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R. W. NEWCOMB,* New York, N. Y. (written discussiont).-On page 1638 mention is made of a new -instrument with an exceptionally high resistance that has been developed by Charles Engelhard. All friction and wear of moving parts of the moving system has been elimi-nated by replacing the hardened steel pivots and jeweled bearings, commonly used on other instruments, by a double metallic filament, one at the top and One at the bottom, under slight tension. Any pos-sible distortion of the moving coil, because of tension, has been eliminated by introducing a solid spindle as the axis of the coil between the points on the coil where the metallic filament is attached. The filaments serve not only as a support for the moving coil; but also to lead in the current from the binding posts to the moving coil, and as a source of counter-torque; instruments so constructed, do not require leveling, and are mechanically very robust. The clock of the recorder serves only to drive the chart at its specified rate and -to operate a small contact-making device; i.e., there is no other mechanical load on the clockworks. The contact-making de-vice is so constructed that there is a quick-make, a quick-break, and a wiping effect while the contact is being made. Contact surfaces on this switch are of platinum platinum-iridium. The operation of this contact, which occurs once each minute, sends a current, from a 6-volt supply; through a solenoid magnet, which operates the depressor bar mechanism in the case of the single-record instrument; in the case of the multiple-record instrument, it operates the automatic switch and color-changing features, as well as the depressor bar.

Jan 12, 1919

By D. Turnbull, J. H. Hollomon

THERE is a large body of evidence'" indicating that solidification during the liquid-solid transition is usually induced by heterogeneities present in the liquid. By dispersing liquid metals into small droplets, the impurities responsible for catalyzing solidification are isolated within a small number of these droplets. The effect of the foreign body therefore is restricted to a single drop by this technique. Thus upon cooling below the melting temperature, solidification is initiated by homogeneous nucleation in the majority of the droplets that do not contain impurities. In the case of solidification of liquid metals, the activation energy for nucleation is so great that its rate changes by orders of magnitude for a change in temperature of only several degrees centigrade.' Effectively homogeneous nucleation occurs at a critical temperature upon continuous cooling. Thus by microscopic observation of single particles during cooling, a temperature at which the rate of homogeneous nucleation becomes sensible can be determined.3 since at the temperatures at which nucleation occurs in the absence of impurities the rate of crystal growth is extremely rapid, the temperature at which the entire particle solidifies is very nearly the temperature at which the nucleation of the solidification occurs. Thus for liquids that freeze at high temperatures the onset of nucleation can be established by simply observing the temperature at which the marked heat evolution and increase in brightness of the particle occur. For liquids that freeze at lower temperatures the onset of nucleation can be determined by a rumpling and change in shape of the particle resulting from its solidification. The microscopic technique for observing the solidification of small particles has already been described." In earlier papers the nucleation of solidification of pure metals 5,6 and of alloy systems7 showing complete liquid and solid solubility have been described. In the present paper, the observations are extended to a simple eutectic system (Pb-Sn) where the possibility of the formation of two solid phases exists. Metals for the investigation were obtained from the American Smelting and Refining Co. in the form of pure lead and pure tin, 99.8 and 99.9 pct purity, respectively. An ingot of each of the pure metals was made into shot by heating the metals at a temperature about 50 °C in excess of the melting point and pouring the liquid slowly into a container of water at 15°C. Samples of the shotted pure metals were weighed out to make alloys containing 5, 10, 15, 20, 25, 30, 40, 50, 60, 70, 80, and 90 atomic pct Pb. Samples of each alloy were then melted in separate beakers. Each melt was poured through a pyrex funnel into a cylindrical mold (% in. ID). The casting solidified in 10 to 20 sec. The inside of the mold as well as the funnel through which the metal was poured were coated with graphite to eliminate adherence of the metal. Analyses were performed on some of the compositions and are given in Table I. The compositions also were checked for these samples and for those that were not analyzed by determining the spread between the liquidus and the solidus upon melting the small metal particles. These measurements agreed as well with the nominal compositions as the analyses listed above. Results The results of the supercooling experiments for the several alloys are summarized in Table II and plotted on the constitution diagram in Fig. 1. Data for the pure lead and pure tin were taken from earlier investigations. The values for the maximum supercooling of the several alloys are the average of several determinations on a number of drops of each alloy. The maximum value in any determination was within about 2 pct of the average. For the alloys containing from 20 to 60 atomic pct Sn, inclusive, two marked changes of the surface structure were observed upon cooling. At the higher temperature, after the first appearance of the solid phase it continued to grow slowly at a constant temperature and then stopped. At the lower temperature the alteration of surface structure was abrupt. For the alloys containing from 70 to 95 atomic pct Sn, inclusive, an abrupt change in surface structure was observed at a single critical temperature.

Jan 1, 1952

By I. Fatt

A recently developed system for measuring electrical resistivity of liquids without use of electrodes offers some interesting possibilities in electric logging technology. The equipment as supplied by the manufacturer is satisfactory for continuous mud logging on a drilling rig or for measuring mud or filtrate resistivity in the laboratory. A simple modification of the commercially available instrument makes it suitable for measuring resistivity of core samples in the laboratory. The continuous measurement of mud resistivity on a drilling rig is a convenient means for detecting mixing of formation water with the drilling mud. Such information is useful to the geologist, the mud engineer and the logging engineer. However, continuous mud resistivity logging by conventional electrode-type resistivity cells is beset with difficulties. The mud, sand and rock chips abrade the electrodes, thereby changing the cell constant and eventually destroying the cell. Also, additives and crude oil in the mud may poison the electrodes by coating them with a nonconductive material. An electrode-type resistivity cell. therefore, may give erroneous readings under certain conditions. Electric logging companies circumvent the electrode poisoning problem by using a four-electrode resistivity cell for measurement of mud resistivity. In this cell, change in electrode area does not change the cell constant. However, the four-electrode cell is difficult to adapt for continuous reading and does not solve completely the problem of electrode abrasion by the sand and cuttings in the mud. The measurement of electric logging parameters on core samples in the laboratory encounters some of the same problems discussed in connection with mud logging. Ideally, the electrical resistivity of a core sample should be measured by placing platinum black electrodes in direct contact with the plane ends of a cylindrical or rectangular sample. Platinum black electrodes however, are much too fragile and easily abraded to be brought in contact with a rock sample. Also, oil or other constituents in the fluid contained in the sample will poison platinum black. In practice, gold-plated brass electrodes, in an AC bridge circuit operating at about 1,000 cps, are used for routine core analysis. For more precise work in research studies, a four-electrode scheme is used.',' Preparation of the samples for the four-electrode method is much too involved for routine core analysis. An apparatus for measuring resistivity of liquids without use of electrodes was described by Guthrie and Boys3 in 1879. They suspended a beaker, containing the electrolyte, by a torsion wire and rotated a set of permanent bar magnets around the vessel. The eddy currents induced in the electrolyte reacted against the rotating magnetic field to develop a torque, which was measured as a deflection of the torsion wire. In 1879 this method could not be made precise or convenient because of the lack of strong permanent magnets. The writer described a very greatly improved apparatus similar to that of Guthrie and Boys, but it was not suitable for continuous measurements or core samples.' Many electrodeless resistivity devices using radio frequency current are described in the literature.5, 6 These generally are suitable only for noting the end-point in a chemical titration. They do not measure resistivity, instead measuring a complex quantity which includes the dielectric constant and the magnetic permeability. The first description of the apparatus to be discussed in this paper was given by Relis.7 Improvements and modifications are described by Fielden,s Gupta and Hills,> and Eichholz and Bettens.10 DESCRIPTION OF APPARATUS The apparatus used in this study is based on the principle that the solution under measurement can form a loop coupling two transformer coils, as shown in Fig. 1. For a fixed AC voltage applied across Coil A, the voltage appearing across Coil B is a function of the resistance of the liquid-filled loop. The details of the voltage generating and measuring circuits are given in Refs. 7, 8, 9 and 10. A block diagram of the equipment is given in Fig. 7. Special features worth mentioning are the operating frequency of 18,000 cps and the automatic temperature compensation which results in the given resistivity readings being automatically correlated to 25°C. The liquid loop supplied by the manufacturer, shown in Figs. 1 and 2, was modified for use in core analysis (Fig. 3). The core sample under test is substituted for a section of the original loop. As shown in Fig. 3, the unit accepts only plastic-mounted cylindrical core specimens. A Hassler-type sleeve easily can be designed for the unit if unmounted cores are to be measured. EXPERIMENTAL PROCEDURE MUD LOGGING A simulated mud line was set up in the laboratory.

By Bob J. Rawicki

TYPES OF WET DUST COLLECTORS Basically, there are two types of wettype dust collectors. One is mechanical, incorporating pumps, motors, fans, sprays, filters, or flooded beds. These come in many forms, but their operating principle is basically the same. The screen or flooded bed is wetted by a series of sprays. Polluted air is drawn in through a fan; here the dust particles impinge on the screen and are flushed off into a settlement tank. The air then passes through spray eliminators to the atmosphere. A great deal of time and money has been spent developing this type of collector. In laboratory tests where clean water at constant pressure, air at constant volume, and dust at low but constant mass to volume were applied, these collectors gave high percentage dust collection efficiencies. Theoretically and technically, they are very good. In practice, however, under rugged mining conditions where there are no constants, and dust load, particle size, water pressure, and volume of air vary with time, their efficiency varies dramatically. Some of the most common problems are: 1. clogging of screens 2. blocking of nozzles 3. replacement. of damaged pump stators Any of the above result in loss of air flow and dust collection efficiency. Generally, there are so many mechanical moving parts, something is always breaking down. This type of collector is very expensive in parts and labor to maintain. The second type of dust collector, which I personally developed, with the help of the British National Coal Board of Great Britain, has none of the above mentioned problems and it works on a completely different principle. My collector, the Mark III Precipitaire Wet-Type Dust Collector, (an improved version of previously successful models) has no internal moving parts, no flooded beds, screens, spray nozzles, etc. It is highly efficient - 99.8% efficiency on total collected dust and 97% on respirable dust. The pressure drop through the collector is constant, hence, air flow remains constant. There is no maintenance expenditure, be it labor or parts. The only maintenance that there is, is desludging. This, of course, varies with the dust load. With a low dust load, desludqinq may only be required every 4 weeks, but this is a very simple operation that can be handled by unskilled men and it takes only a very short time. My collector is powered by a ventilation fan that is placed on the clean air side for a longer fan and motor life. Dust is extracted solely by water action. The collector's operating principle is: Dust laden air is drawn in along ducting into a tapered scrubber section, shaped to create a self-induced curtain of water. This action washes the dust particles from the air and the collected dust settles into the bottom of the tank. Cleaned air is then exhausted via a series of spray eliminators where it is completely dried and on into the atmosphere. These collectors have been sold in Great Britain, to the National Coal Board, and throughout Europe. They have been working very well for many years now. GENERAL APPLICATIONS Dust is very dangerous; silicosis and black lung kill and disable many workers each year. Many of the mine explosions can be attributed to coal dust. By the use and application of dust collectors, these deaths and disasters can be avoided. There really is no excuse. However good and efficient a dust collector may be, it's positioning and installation arrangement is critical. The collector may remove 99% of dust supplied to it, but it takes the skill and experience of a dust control engineer to design and fit ducting, hoods, etc. to remove polluted air at source and deliver it to the collector. In some cases this is very simple; in the case of longwall machines, it is very difficult. In general, dust collectors should be used to collect dust at every point of dust generation. I have noted a great reliance on dilution as a means of dust control. I personally think this is a dangerous and unreliable method. As mines become deeper and the use of larger and more productive equipment becomes more common, reliance on dilution will be impossible and dust collectors will be essential.

Jan 1, 1982

By Lyall, Zickrick

As a result of the studies on recrystallization and crystal growth made in this laboratory, certain theories have been developed. These are expressed briefly in a paper by Dean and Hudson.' One of the principal points brought out in that paper is that in the deformation of a crystal, the energy supplied is distributed to the atoms of the lattice, probably by the forced formation of molecules. It is found that a Maxwellian distribution of the energy among these atoms will account for the grain growth at various temperatures. According to such a distribution the number of atoms with energy above a certain critical value, E, necessary for recrystallization at the absolute temperature T is given by n = Ne-E/kT where N is the total number of atoms. It is apparent that if this line of reasoning is correct, a metal which has been cold-worked and reheated to a temperature below that of complete annealing will have the atoms with the higher energy recrystallized, that is, reduced to normal energy and there will remain only atoms below a certain energy. If this metal is again cold-worked the peak in the number-energy distribution curve will, as compaied with its position after the first cold-working, be displaced toward the regions of lower energies, that is, the temperature of recrystallization will be higher. By a repetition of this process the position of this maximum and hence the recrystallization temperature of the metal could be raised considerably. In order to check this theory, experiments have been made on copper wire. The wire was drawn from 1/4-in. rod to 22 B & S gage and then sample lots were annealed at 400 and 220° C., respectively. The wire annealed at 400° C. gave an elongation of 34 per cent., whereas that annealed at 220° C. gave only 23 per cent. These wires were then drawn by identical practice to 34 B & S gage and the elongation determined after an anneal of 3 min. in an oil bath held at various temperatures. The figures obtained have been plotted in Fig. 1. It will be seen that the

Jan 1, 1927

By P. C. J. Gallagher

A number of recmt determinations for the ratio of extrinsic to intrinsic stacking fault energy in fcc solid solutions are examined. Some of these arise from incomplete analyses which can yield only approxi?nate values for the ratio. Reliable results, on the other hand, obtained using extrinsic-intrinsic fault pairs, show that the extrinsic and intrinsic fault energies are essentially equal in several materials. There is some reason to believe that this finding is of general applicability to fcc elements and alloys. A wide range of values has been obtained for the relative magnitudes of the extrinsic and intrinsic stacking fault energies (yext and yint, respectively) in recently published studies in a variety of materials. In contrast, Hirth and Lothe' using a central force model have shown that out to tenth nearest-neighbor interactions the perturbation in energy caused by both types of fault is the same. Although the model used is not completely valid in metals, there is nevertheless some indication that marked variations of yext/nnt should not be observed from one material to another. In early work in Cu-A1, Cu-Ge, Ni-Co, and stainless steel all the deformation faults observed in the electron microscope were found to be intrinsic in nature, which led to an attitude that the extrinsic fault energy must be considerably greater than the intrinsic. Extrinsic faulting arising from deformation has, however, more recently been directly observed in Au-4.8 at. pct n;~ Ag-6 at. pct Sn and Ag-8 at. pct sn; Ag-7.5 at. pct In and Ag-11.8 at. pct 1n;"' pure silwer and Ag-0.5 at. pct ~n;' and Cu-22 at. pct Zn, Cu-30 at. pct Zn, and Cu-7.5 at. pct ~1.l' Multilayer loops containing extrinsic faulting have also been observed in quenched aluminum." While peak asymmetries in X-ray faulting probability studies were generally attributed to the presence of twins,Lelel2 has recently reinterpreted earlier X-ray data in Ag-Sb alloysU in terms of the presence of extrinsic faulting. The determinations of yeXt/yint made from the above studies are shown in Table I, with a brief description of the techniques employed. A number of the methods utilized are deficient in one or more respects, and the reliability of the values listed will be discussed. ~ele'~ recognizes that his approximate determinations of yext/yint assumes equal numbers of extrin-sically and intrinsically faulted dislocations. It is well-known, however, that such an assumption is not at all justified since extrinsic faulting has but rarely been observed in samples studied in the electron microscope. The only conclusion that should be drawn from the X-ray results at present is that the total intrinsic scattering cross section (i.e., the product of the width of the intrinsically faulted dislocations with their density) is approximately ten times greater than for extrinsic faulting in these particular samples. An important point is that the relative magnitudes of the energies cannot be inferred from results of this type, unless the intrinsic and extrinsic faults form with equal ease. One must recognize that, although a formation barrier may restrict the amount of extrinsic faulting which occurs, this in no way implies that the extrinsic and intrinsic energies should be different. It is unlikely that a worthwhile estimate of the relative densities of extrinsically and intrinsically faulted dislocations can be made at the high deformations present in X-ray samples. ~oretto,'~ from a statistical argument applied to the nonobservation of extrinsically faulted tetrahedra out of a large sample, concluded that yeXt/yint could not be less than -4.5. However, the present author feels that a high-energy formation barrier as just supposed also explains this finding satisfactorily and that no conclusion can possibly be drawn concerning the actual extrinsic stacking fault energy. The same argument also serves to explain the fact that extrinsic faulting has been relatively little observed in the electron microscope. Extrinsic-intrinsic node pairs and isolated extrinsic nodes were first reported by Loretto~ and subsequently by Ives and Ruff,' Gallaher,' and Gallagher and Wash-burn.' Ives and Ruff' found a wide spread in the ratio of extrinsically to intrinsically faulted area in the node pairs they observed, and drew the very tentative conclusion that yeXt/yint 2 2. They recognized that a straightforward comparison of the size of the faulted areas could provide no more than a qualitative result without a theoretical analysis of the dislocation geometry associated with extrinsic faulting. A theoretical

Jan 1, 1969

By J. C. METCALF

MORE than 80 per cent. of the iron produced in the United States and over 30 per cent. of the world's annual production is obtained in the Lake Superior district. Though iron ore was discovered on the Marquette range in 1844, the poor transportation facilities retarded the development of this region for many years. The structure of the Lake Superior basin is essentially an east-west synclinorium with steep dips on the south side of the lake and considerably flatter ones on the north and west. The Upper Huronian series, which -is the iron-bearing one of the formation, on the south side of the lake dips north from 55' to 80°, and on the north side dips south from 8" to 200. The series has been subjected to local folding and faulting, which have influenced the development of the mining systems used.

Jan 1, 1921

By F. G. Smith

A few years ago, the writer encountered a problem that, at first, seemed to be due to peculiar conditions affecting grain growth. Large cups made from heavy metal failed in the first drawing operation in the process of making seamless tubes. The metal, as cast, appeared to be sound and strong; it rolled successfully and withstood the first cupping operation, but on the first draw it failed, with a crystalline fracture. The failure appeared in the slightly worked part of the bottom of the cup, and microscopic examination revealed exceptionally large grains. Knowing the general conditions governing recrystallization of brass, which were later published by Mathewson and Phillipsll an investigation was outlined with the idea of including various conditions under which new grains might form, and which would include the effect that a previous anneal might have upon the anneal following. These conditions were produced by annealing specimens of brass at five different temperatures, indenting them with a 10-mm. ball under four different pressures, and then reannealing at each of the five temperatures five specimens each of which had been annealed at one of the five temperatures. Preparation of Specimens The material used was cartridge brass 0.400 in. thick, having the following composition: Copper 66.60 per. cent., zinc 33.35 per cent., lead 0.02 per cent., iron 0.03 per cent. This was rolled with 35 per cent. reduction after a 700" C. anneal. Fig. 1 shows the structure of this original bar on which all subsequent anneals were made. Pieces 1 in. (2.5 cm.) wide and 3 in. long were prepared and annealed for 1/2 hr. at 450°, 550°, 650°, '750°, and 850" C. Each of these pieces are indented under the Brinell test with a 10-mm. ball at 500, 1000, 2000, and 3000 kg. pressure. Then, sets of five pieces from each of the original anneals were reannealed at 450°, 550°, 650°, 750°, and 850" C.

Jan 1, 1921

By Kenneth Schellinger

THE terms surface tension and surface energy are well known when applied to liquids and are generally described by referring to the excess energy of the air: liquid interface as a result of unsaturated molecular forces surrounding the surface molecules of the liquid due to the presence of the air phase on one side. Such unbalanced forces produce the familiar water droplet of spherical form and are generally summed up as a surface tension measured in dynes per centimeter which can be shown mathematically to be equal numerically to a corresponding surface energy expressed in ergs per square centimeter. A specific surface energy, however, is best thought of as the energy necessary to produce one unit, of new surface on a substance. Hence, in producing a bubble in a flotation cell the impeller must supply surface energy corresponding to the air: liquid interfacial area on the interior of the bubble. Inasmuch as it is relatively easy to extend or contract the surface of a liquid, there are a number of successful methods for liquid surface tension, or energy, measurement based upon surface deformation. This happy state of affairs does not, however, extend to solids, which are considered to possess surface energies for the same reasons as do liquids, i.e. because of unsaturated ionic bonds at the solid: gas interface. As in the case of the flotation cell producing surface on liquids as new bubbles, it takes energy to produce new surface on solids as new particles. As every mill man knows, this surface is produced on mineral solids in a grinding mill by the action of a tumbling mass of iron balls. But here so much energy usually is wasted by the inefficient action of these balls that a large amount of heat is generated, and the surface energy production may be easily confused with the energy necessary to produce this ineffective heat. The tumbling balls and fracturing minerals ultimately take their energy from a rather large electric motor. It has been variously estimated that from 10 to 20 pct'" only of this energy from the motor does not appear as heat and may be presumed to appear as surface energy on the min- erals present. Such a production of new surface on the mineral phases is accompanied, of course, by a size reduction that is inevitable as more and more mineral interior molecules become surface molecules by the fracture exposure. This size reduction of mineral particles, although the most obvious feature and perhaps the sole object of the milling operation, is from this energy viewpoint the outward manifestation of the production of surface energy only. Measurement of the characteristic surface energies of pure minerals and their various mixtures in ores would be a step towards understanding of the energetics of the commercial grinding operation. In addition, the characteristic surface energy of a mineral is probably a physical property specific for that mineral, and therefore, from a scientific standpoint, should be measured. It is interesting to note that, in contrast to the large body of work on the surface tensions of liquid systems and biological systems, the field of solid surface energies has been neglected. Prior to 1920 it is difficult to find more than one or two references to work on solid surface energies in Chemical Abstracts. Since 1920 such references number somewhat less than 100, while those on liquid systems are numbered in the thousands. Much of this apparent neglect of the field of solid surface energies (the term is intended to be somewhat inclusive at this point and refers both to the solid: gas, and the solid:liquid interface) is because of the lack of a reliable method of measurement rather than any lack of scientific curiosity. It was, and still is, difficult to produce new surface on a solid without the simultaneous production of interior changes in the same solid which may consume part of the energy used. The extension in the surface area can be measured, but the interior crystal-

Jan 1, 1953

By Kenneth Schellinger

THE terms surface tension and surface energy are well known when applied to liquids and are generally described by referring to the excess energy of the air: liquid interface as a result of unsaturated molecular forces surrounding the surface molecules of the liquid due to the presence of the air phase on one side. Such unbalanced forces produce the familiar water droplet of spherical form and are generally summed up as a surface tension measured in dynes per centimeter which can be shown mathematically to be equal numerically to a corresponding surface energy expressed in ergs per square centimeter. A specific surface energy, however, is best thought of as the energy necessary to produce one unit, of new surface on a substance. Hence, in producing a bubble in a flotation cell the impeller must supply surface energy corresponding to the air: liquid interfacial area on the interior of the bubble. Inasmuch as it is relatively easy to extend or contract the surface of a liquid, there are a number of successful methods for liquid surface tension, or energy, measurement based upon surface deformation. This happy state of affairs does not, however, extend to solids, which are considered to possess surface energies for the same reasons as do liquids, i.e. because of unsaturated ionic bonds at the solid: gas interface. As in the case of the flotation cell producing surface on liquids as new bubbles, it takes energy to produce new surface on solids as new particles. As every mill man knows, this surface is produced on mineral solids in a grinding mill by the action of a tumbling mass of iron balls. But here so much energy usually is wasted by the inefficient action of these balls that a large amount of heat is generated, and the surface energy production may be easily confused with the energy necessary to produce this ineffective heat. The tumbling balls and fracturing minerals ultimately take their energy from a rather large electric motor. It has been variously estimated that from 10 to 20 pct'" only of this energy from the motor does not appear as heat and may be presumed to appear as surface energy on the min- erals present. Such a production of new surface on the mineral phases is accompanied, of course, by a size reduction that is inevitable as more and more mineral interior molecules become surface molecules by the fracture exposure. This size reduction of mineral particles, although the most obvious feature and perhaps the sole object of the milling operation, is from this energy viewpoint the outward manifestation of the production of surface energy only. Measurement of the characteristic surface energies of pure minerals and their various mixtures in ores would be a step towards understanding of the energetics of the commercial grinding operation. In addition, the characteristic surface energy of a mineral is probably a physical property specific for that mineral, and therefore, from a scientific standpoint, should be measured. It is interesting to note that, in contrast to the large body of work on the surface tensions of liquid systems and biological systems, the field of solid surface energies has been neglected. Prior to 1920 it is difficult to find more than one or two references to work on solid surface energies in Chemical Abstracts. Since 1920 such references number somewhat less than 100, while those on liquid systems are numbered in the thousands. Much of this apparent neglect of the field of solid surface energies (the term is intended to be somewhat inclusive at this point and refers both to the solid: gas, and the solid:liquid interface) is because of the lack of a reliable method of measurement rather than any lack of scientific curiosity. It was, and still is, difficult to produce new surface on a solid without the simultaneous production of interior changes in the same solid which may consume part of the energy used. The extension in the surface area can be measured, but the interior crystal-

Jan 1, 1953

By B. Foley

IN THE first report1 disks of steel of known composition and history were exposed, under carefully prescribed conditions, to impacts of explosion products resulting from the explosion of 50-gm. charges of explosives having well-determined rates of detonation, or to impacts of a weight of known mass, falling through measured distances. There were available at the Bureau of Mines Experiment Station five explosives, having rates of detonation of 5716, 4470, 3190, 2296, and 1523 meters per second. It being desired to continue this exposure downward, and no explosives with a lesser rate of detonation being at hand, resort was had to the impact of a falling weight, the differences in the velocity of impact being attained by varying the height from which the weight was allowed to fall. It was expected by this means to demonstrate experimentally that the development of Neumann bands was determined by the suddenness of the deformation of the metal in which they were produced. But while progressive deformations were obtained with the explosive arges, the falling-weight method failed because the tup was ogressively deformed, also the disks were so flattened as to be unfit for metallographic examination. A return, therefore, has been made to the use of explosives as the source of energy, an air-gap being interposed between the charge of explosive and the disk, as the effect diminishes as the function of the distance between the charge and the object on which the products of its explosion, or the shock wave from its detonation, impinge. The details of the arrangement of the tests by the air-gap method were the same as those described by Foley and Howell,2 except that after the system had been set up and the desired apparent specific gravity for the explosive

Jan 2, 1926

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

By ALFRED KAUFFMAN

NO matter what position we hold, workman, foreman, superintendent, manager, president, or what not, let us fail to give or to make good products, then see how quickly we'll be called to account for- our work by the buying public. The waves of progress taught us that millions were wasted in unnecessary strikes-we also learned that many losses were due to neglect on the part of manufacturers to give the same consideration and attention to the human element of their factory as they gave to their machinery. The employees learned also that the employer was their agent who found purchasers for the product of their labor. So between the two we learned that many years of labor were needed in order for a worker to recover his wasted savings, or for the manu¬facturer to replenish his loss. Treat 'em rough, and tell 'em nothing, was not very far from the true relationship between management and employees in manufacturing plants in the early days. Today just exactly the opposite views are held by executives whose function is the handling of employees. Men today want to know what it is all about. They are intelligent enough to comprehend the facts, and to use them constructively, and it is good business to give them the information.

Jan 1, 1929

By Orson Cutler, Shepard

THE OBJECT of this paper is twofold: (1) To analyze the forces that cause air bubbles to spread on mineral surfaces in the flotation process; and (2) To develop a rational expression that will serve as a criterion of the floatability of minerals, to the end that the efficiencies of various flotation reagents can be accurately compared. Heretofore, the subject of the spreading of air bubbles has been dismissed with the statement that the surfaces of minerals on which bubbles spread are water-repellent. Imperfect understanding of the forces involved has led to the use, hitherto, of various erroneous formulas for the calculation of the comparative effectiveness of flotation reagents.

Jan 1, 1932

By ED. E. Furman, R. H. Atkinson

HITHERTO the practical creep testing of precious metals has received little or no attention. The only previous creep tests of precious metals have been made with wires under conditions such as to yield much more rapid rates of creep than in engineering tests.', ' Up to the present time the value of creep bars of adequate size, in the absence of real need for engineering data, has deterred investigators. However, the increasing use of platinum at high temperatures has demonstrated the need for reliable creep data for the guidance of engineers, especially those engaged in designing certain specialized chemical plant equipment. In order to supply this need, creep tests were conducted at 1382°F (750°C) on 0.290 in. diam specimens of platinum, 90 pct Pt, 10 pct Rh and palladium. The platinum was high purity, nominally 99.95 pct Pt. The 90 pct Pt, 10 pct Rh was of the same high quality as is used for making gauzes for the catalytic oxidation of ammonia. The palladium was also of high purity; two batches of palladium bars were tested, one deoxidized with calcium boride and the other with aluminum. Spectrographic examination of the palladium confirmed its good quality; the only significant impurities apart from the residual deoxidizers were traces of silicon and lead. Procedure The creep bars, which were furnished by Baker and Co. to our specification, were 6 ¾ in. in overall length with a 4½ in. (4 in. gage length) reduced section 0.290 in. in diam and had the ends threaded (?-NC16). It may be of interest that the bars were valued at up to $600 each. The specimens were supplied in a 50 pct cold-worked condition to facilitate attachment of the creep extensometer, which was of the push rod type. Because of the softness of the platinum and palladium, the extensometer rings were secured to the test section by means of circular knife edges instead of the usual pointed set screws. The extensometer rods extended through the bottom of the furnace and readings were taken with a 0.0001 in. "Last Word" dial gage fastened to the rods for the duration of the test. The bars were directly loaded by hanging weights from the lower specimen grip. All tests were conducted at 1382°F ± 2°F, and an effort was made to maintain the temperature gradient over the test section within 2°F. The ends of the furnace tube were packed with asbestos wool, which allowed a very slow circulation of air through the tube. Annealing was accomplished in the creep furnace before the load was applied. The platinum and palladium specimens were annealed at the test tem- perature for about 17 and 24 hr respectively; in the case of the rhodioplatinum it was found expedient to anneal for 1 hr at 1922°F (1050°C). Pilot samples cut from the same stock as the bars were used to check annealing procedures. Pertinent measurements of grain size and hardness were recorded. Results and Discussion The creep data obtained are given in Table I and the creep curves are plotted in Figs. 1, 2, and 3. Two platinum specimens, tested under a stress of 250 psi, had almost identical creep rates at 2000 hr, namely 0.000008 and 0.000009 pct per hr. A third platinum specimen, stressed at 400 psi, had a creep rate at 2000 hr of 0.000026 pct per hr; the reason for a rather sharp decrease in creep rate during the period from 1200 to 1600 hr is unknown. As it was thought that 90 pct Pt, 10 pct Rh would have a lower creep rate than platinum, the first sample was tested at 400 psi; however, the creep rate was approximately 50 pct greater. Microex-amination revealed that differences in grain size might be responsible for the unexpected result, as annealing at 1382°F developed an average grain diameter of 0.0021 in. in the rhodioplatinum specimen compared with 0.004 in. in the platinum bar. Annealing the alloy for 1 hr at 1922°F (1050°C) increased the average grain diameter to 0.0032 in. and materially improved the creep resistance, making it much better than platinum. A second specimen annealed at 1922°F (1050°C) and tested under a stress of 550 psi had a creep rate of 0.000022 pct per hr at 2000 hr, which was still substantially lower than that shown by the specimen annealed at 1382°F (750°C) and stressed at only 400 psi. In contrast to the creep behavior of the platinum and rhodioplatinum specimens, the palladium bars, whether deoxidized with calcium boride or aluminum, were characterized by high first stages of creep. However, after about 1200 hr of test, the creep

Jan 1, 1952

By H. E. Stauss, J. Hino

INTEREST in silicon has arisen again in the past decade as a result of improvements in crystal rectifiers.' Although the preparation of silicon was first reported by Berzelius in 1880, the early product was of relatively low purity, and only the need for rectifiers in World War II led to the production of a 99.9+ pct pure powder. This material in crystalline form was consolidated into massive silicon for use, and the method developed was to melt it with selected added constituents as "doping" agents. Melting techniques, therefore, are of great importance. There are two basic problems in producing silicon ingots free of doping additions; one is the prevention of spitting and the other is prevention of cracking of the ingot during freezing. The most satisfactory arrangement yet developed for producing massive silicon is to melt and freeze in a cylindrical quartz crucible surrounded by a concentric heating element and concentric radiation shields or insulation. For example, use can be made of a tubular heater with a high frequency generator as the source of power and reflecting shields of alundum cylinders. The spitting of silicon is related to gas evolution, and the gas comes from two primary causes—adsorbed gas and the reaction products of silicon and the crucible. Gas is also released from bubbles contained in the quartz crucible walls. Improved removal of adsorbed gas can be achieved by means of controlled melting and freezing. The seriousness of the problem in vacuo is reduced with an electrically operated mechanical movement of the high frequency power coil. The upper portion of the powder charge is melted first and the high frequency coil lowered until the powder is completely molten. During cooling the high frequency coil is raised slowly. These means also reduce the final nonviolent extrusion of large beads of metal through the ingot top during freezing. Better control of spitting and bead extrusion is obtained when melting is done under helium at. atmospheric pressure instead of in vacuo. The problem of reaction between silicon charge and crucible in practice is confined to the reaction between silicon and quartz. This2 apparently is: Si + SiO2 + 2SiO The part that this reaction plays in spitting has not been isolated for separate study. SiO is a volatile vapor at the melting point; of silicon and is released freely during melting in vacuo, but hardly at all in helium at atmospheric pressure. The cracking of ingots is a major difficulty in melting silicon, and its prevention requires special melting techniques or the addition of "toughening" agents such as aluminum or beryllium.' The cracking of the ingots has been explained as being the result of the expansion that occurs upon freezing; although direct observation of freezing ingots reveals visible cracks on the surface only after a red heat has been reached, suggesting that cracking is the result of differential contraction of silicon and quartz. Silicon wets quartz, and the ingot adheres tightly to the crucible. Therefore as ingot and crucible cool, the two either have to pull apart, or at least one must crack. Surprisingly, in spite of the relative thinness of the quartz and the thickness of the ingot, the ingot and the crucible both crack. Microscopic and X-ray4 studies fail to show any plastic flow other than twinning in the ingots. Slow cooling fails to prevent cracking. Another possible solution to cracking is to weaken the crucible. Use of thin-walled crucibles finally led to success with fused quartz crucibles with a wall thickness of 0.25 to 0.50 mm. With such thin-walled fused quartz crucibles consistently uniform success is secured in producing sound ingots 30 mm in diam from the purest available grade of silicon (99.9+) without the use of any type of addition. Melts are made in the size range of 50 to 100 g. Omission of a deliberately added doping agent is not sufficient to insure pure ingots. The reaction of silicon with crucibles and the resultant solution of impurities in the silicon is well-established." In this laboratory, the presence of Al, Be, and Zr has been found spectroscopically in ingots melted in contact with alumina, beryllia, and zircon. The best crucible materials reported in the literature are MgO and SiO2. Use of MgO in this laboratory has resulted in a heavy deposit of magnesium on the furnace walls, showing that a reduction of the magnesia occurred and the resulting magnesium removed from the melt by volatilization. In the case of quartz, the silica is reduced and SiO liberated to deposit on the equipment walls. There probably is real danger that oxygen is dissolved in the ingot when either magnesia or silica is used as the crucible material. Preliminary analyses by Dean Walter in his vacuum unit in this laboratory6 indicate the presence of oxygen in undoped silicon melted in quartz.

Jan 1, 1953

By G. F. Leaming

The paper by R.V. Ramani and R.J. Sweigard is a wonderful description of the labyrinthine web that has been spun about the mining industry by energetic bureaucrats and politicians over the past 50 years. The remedy for the problem, however, is not more of the same, but less. That may be difficult for the industry to achieve, for it is not a technical solution but a political one. And the current fervor for more detailed planning at all levels of government and private enterprise has become deeply ingrained. The authors recommend the provision of more information about mining and mineral resources to "macro" (i.e., government) land use planners. They apparently overlook, however, the already strong tendency on the part of most government land use planners to consider themselves omniscient. Thus, giving them more information about the technical problems of mining will only make them want to get more and more involved in the "micro" (private, site specific) mine development and production plans of the individual mining firm. In fact, this has already happened at all levels of jurisdiction from municipal to federal government. Examples are legion. The most effective way to ameliorate the adverse impacts of government land use planning on existing and potential mining operations is to: (1) introduce greater flexibility in the definition of land use zones by local and state governments; (2) adopt realistic and relevant ambient environmental performance standards in governing relationships between mineral land uses and concurrent or subsequent nonmining land uses; (3) allow greater leeway for economic considerations in land use decisions in contrast to the explicit legalistic approach now in vogue; (4) recognize that all minerals are not the same and that sand and gravel mining should not be treated the same as underground metal mining, coal stripping, oil field production, or in situ leaching; and (5) eliminate the notion that mining operators should be responsible for determining in detail the use of land by subsequent owners of mined land. This last bit of conventional ethic really makes no more sense than requiring the builders of every shopping center or government office complex to provide detailed plans for the use of that land when its use for shopping or government is ended. Did the builder of Ebbetts Field plan for Brooklyn after the Dodgers went to Los Angeles? Should the developer of the Bingham Pit plan for suburban Salt Lake City after the copper mining goes to Chile? The nation's mining industry must address these questions before further bankrupting itself to provide more data to planners and spending thousands of dollars per acre to create land that when reclaimed is worth only a few hundred dollars per acre. ? Reply by R.V. Ramani and R.J. Sweigard We thank Mr. Learning for his valuable contribution. His views on the problems of land use planning and mineral resources are most welcome additions to our paper. As the title indicates, our paper was more concerned with the impacts of land use planning on mineral resource conservation than with the details of the planning process. On the whole, his five recommendations would be helpful for mineral resource conservation. However, we would suggest that the argument he presents for his final recommendation does not address the differences between mining as a land use and commercial or institutional uses. We believe that this difference is the crux of the issue. We share Mr. Learning's desire to ameliorate the adverse impacts of land use planning. Possibly the most detrimental impact is the loss of mineral resources. Any development, whether mineral or community, that does not give proper consideration to other resources can result in permanent loss or sterilization of resources. With proper planning, some of these losses can be avoided. As our paper indicated, one factor that limits the consideration of mineral resources, and ultimately leads to their sterilization, is the generally inadequate levels of resource characterization and understanding of the unique nature of mineral resources and mining operations. The last point raised by Mr. Learning is also important. In terms of reclamation and land use planning in mining districts, we certainly do not advocate spending more than what the results are worth. The main thrust of the paper was to explore the avenues for conserving the mineral resources so that, at some appropriate time, the issue of mining and reclamation can still be addressed. ?

Jan 1, 1986

By Arthur B. Foote

THE ball mill has superseded stamps for the reduction of gold ores in most of the recently designed plants, partly because stamps are not suited to die fine grinding required for flotation, and partly to save space and construction cost. Experience with these new mills seems to confirm the idea that it is more difficult to recover bold from a ball-mill product than it is when stamps are used for crushing. Microscopical examination of particles of gold that have passed through a ball mill show that the gold has been pounded into exceedingly thin flakes coated with a talcy surface, making it more difficult to save by amalgamation, flotation, or concentrating. Bearing in mind that gold is extremely malleable, it seems reasonable that this should be so. Contrast the action in a stamp battery, where the crushing is by impact in the presence of mercury, to the grinding and rolling under pressure in a ball mill. It is well known that a better recovery can be obtained by panning or amalgamation from a sample of ore that has been crushed by mortar and pestle than from one reduced on a bucking board.

Jan 1, 1937

By Stanley L. Lopata, Eric B. Kula

SEVERAL methods are available for determining pole figures by X-ray means.' The earlier film methods have been replaced by techniques in which the intensities are measured by Geiger counters on an X-ray diffractometerZm7. These methods utilize either flat transmission or reflection samples,214°8 cylindrical specimens,3 or spherical specimens.7 A single transmission or reflection sample will not yield information over the complete pole figure. The cylindrical specimens suggested by Nortod and the spherical specimen of Jetter and Borie7 have the advantage of allowing the whole pole figure to be obtained without any corrections to the intensity for absorption, There is a lower limit to the size of sheet which can be conveniently studied, however, and sample preparation can be rather tedious. Probably the most common method today for determining the complete pole figure is that developed by Schulz. A flat reflection sample is used for determining the pole figure from the center out to about 70". Because of the geometry of the system used, little or no correction for absorption or irradiated volume is necessary.4'6 A separate transmission sample is used for the region near the edge of the pole figure. This procedure requires two separate samples, one of which must be a thin carefully-prepared transmission sample. Furthermore, since the reflection and transmission data are in different arbitrary intensity units, a region of overlap must be obtained, and the intensity data from one set of measurements converted to units of the other. These are serious disadvantages of this method, and they point out the need for a simplified procedure. Since the reflection technique can be used for planes whose normals lie up to about 70° from the sample surface normal, it is apparent that a complete pole figure can be obtained by reflection alone if sample surfaces are cut at oblique angles to the rolling plane Specifically, if a rolled sample is cut so that the normal to the surface formed lies equidistant (54" 44') from the rolling plane normal, rolling direction, and transverse direction, then complete information for one quadrant of the pole figure can be obtained by reflection from the surface. Fig. 1 shows this oblique surface, as well as the position of the pole of this surface in the pole figure. When a surface has been cut oblique to the rolling plane, the standard polar stereographic net is inconvenient to use, and it would be more desirable to have the center of the net coincide with the pole of the oblique plane. Fig. 2 shows such a net, where the center has been offset 54' 44' to correspond to a specimen cut as in Fig. 1. This net was in effect obtained by rotating a standard polar stereographic net 54" 44' with the help of a Wulff net. With the experimental setup used. a sample can be cut from plate of 1/2-in. thickness or br Gen- erally thinner sheet is under investigation, and a composite specimen must be used. A convenient procedure has been to bond together, using epoxy resin, sufficient sheets to form a cube. These are clamped in a vise, and when dry, the whole vise is rotated and a flat surface ground at the required angle. The sample is then mounted inside a larger steel ring using Koldmount, the backside ground flat and parallel to the approximate desired thickness. The sample is then polished and etched to remove any effects of cold working during grinding. With this method only one quadrant of the pole figure is obtained. Often pole figures show symmetry around the rolling and transverse directions, and any slight asymmetry is due to scatter. Should the pole figure not be symmetrical, four oblique surfaces, corresponding to the four quadrants of the pole figure, would have to be examined. In most cases there is symmetry at least around the rolling direction, which reduces to two the number of quadrants to be investigated. For many purposes all that is required is an average polefigure for the four quadrants. This canreadilybe obtained with composite specimens of sheet material, where sheets Corresponding to each of the four quadrants can be intermixed. The four quadrants can be obtained by considering sheet in the normal position, and by rotatiolls of 180" around the sheet normal, the rolling direction, and the transverse direction. If desired, the whole thickness of the sheet can be used, yielding an average of the surface and interior textures; or the surface material can be removed from each sheet, resulting in a pole figure for the center alone. Eugene S. Meieran of the Massachusetts Institute of Technology has independently developed the same method. His results, adapted to a pole figure goniometer with a specimen spiraler, will be described in another publication.

Jan 1, 1962

By Edgar M. Dunn

Part I. Determination oF Gases in Smelter Flues. General considerations. Regular methods for carbon monoxide, oxygen, nitrogen, moisture. Sulphur oxides-—Methods of Lunge and Hempel tried, and either modified or discarded, with reasons therefor. Gravimetric method developed at Anaconda. Description of apparatus used. Brief notes on Richter and Hawley methods for the direct cietermination of sulphur trioxide. Carbon dioxide, with complete notes on same. Arsenic trioxide. Table of percentages of flue gas constituents found at a Western smelter. Some final notations as to the value of flue gas analysis, in connection with an intelligent log of furnace operations. Part II. Notes on the Determination oF Dust Losses at the Washoe Reduction Works, Anaconda, Mont. Discussion of problem, with description of flue system. Various places and methods for determinations of velocity. Instruments used. Procedure in making determinations for velocity. Soundings of cross-section for depths of dust. Calculation of velocities and areas. Daily volume of gas, and plant operations during tests. Place for dust determinations. Apparatus and methods of 'sampling. Results obtained, with table of daily amount of dust losses. Analysis of dusts for values, from various sampling stations. Complete analysis of composite sample of stack emanation. Last analysis totaled to show form in which present. Discussion of recovery as a commercial proposition. References on Pitot tube and calculations.

Jan 1, 1914