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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 P. R. Kalischer

IN the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more components that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. Since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measurements and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. NATURE AND REMOVAL OF SURFACE BARRIERS The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 per cent Fe, 50 per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However, this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By Ralph Hultgren, Bernard York, David W. Mitchell

It is a well-known fact that magnesium-alloy castings are apt to be coarse grained if the melt is not superheated several hundred degrees above the melting point before casting. (The casting temperature varies according to the shape of the mold. A typical casting temperature is perhaps 1400°F.) British practice is to heat to 900°C. (1650°°F.) for 15 min., cool rapidly to casting temperature, and cast.1 In Germany superheating is carried out at 850° to 900°C. (1560° to 1650°F.) depending on the amount of scrap used. It is stated that further refinement will be obtained by prolonging the period of superheating or by increasing the superheat temperature to 950°C. (1740°F.).2 In the United States superheating is carried out at i600° to 1700°F. (871° to 927°C.), perhaps even higher in some places. It is stated that superheating effects are found as low as 1500°F. (816°C.), but several hours are required.3 These commercial treatments lead to grain sizes in sand castings that may vary from 4 to 8 grains per sq. mm.§ in heavy sections and from 60 to l00 in 3-in sections to perhaps 380 in thin sections. It is also generally known that the refining effect of superheating is lost if the melt is held for some time at lower temperatures before casting. Aside from these very qualitative statements, there is little to be found in the literature as to the effect of temperature and time of superheat on the final grain size. Because of the uncertainty of these factors, the Office of Production Research and Development of the War Production Board placed a research contract with the University of California, supervised by the War Metallurgy Committee. This research, which was done under the "Restricted" Project NRC-550, is the basis of this paper, which has been released for publication by the O.P.R.D. The material studied was an alloy prepared from carbothermic magnesium. The temperatures required for grain refinement proved to be widely different from those used in practice, as described in the statements in the first paragraph. This difference is attributed to the fact that the magnesium in the specimens was of carbothermic origin instead of the electrolytic magnesium in common use. MATERIALS AND METHODS The magnesium alloy studied was one of the most popular sand-casting alloys, with a nominal composition of 9 per cent aluminum, 2 per cent zinc, and 0.r per cent (minimum) manganese and the balance magnesium. This is designated

Jan 1, 1945

By P. R. Kalischer

IN the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more components that tend to form very stable oxides Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken If, however, it s required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible Since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets All of the pertinent properties of the magnets could be accurately and delicately measured by density measurements and magnetic tests of sufficient scope to give a complete demagnetization curve From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties NATURE AND REMOVAL OF SURFACE BARRIERS The early work of the present investigation was based upon published processes In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 per cent Fe, 50 per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200ºC or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics However, this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen Both the iron and nickel powders sintered

Jan 1, 1941

By Ralph Hultgren, Bernard York, David W. Mitchell

It is a well-known fact that magnesium-alloy castings are apt to be coarse grained if the melt is not superheated several hundred degrees above the melting point before casting. (The casting temperature varies according to the shape of the mold. A typical casting temperature is perhaps 1400°F.) British practice is to heat to 900°C. (1650°F.) for 15 min., cool rapidly to casting temperature, and cast.' In Germany superheating is carried out at 850' to 900°C. (1560° to I650°F.) depending on the amount of scrap used. It is stated that further refinement will be obtained by prolonging the period of superheating or by increasing the superheat temperature to 950°C. (I740°F.).2 In the United States superheating is carried out at 1600' to 1700°F. (871' to 927°C.), perhaps even higher in some places. It is stated that superheating effects are found as low as 1500°F. (816°C.), but several hours are required.3 These commercial treatments lead to grain sizes in sand castings that may vary from 4 to 8 grains per sq. mm.! in heavy sections and from 60 to IOO in 1/2-in. sections to perhaps 380 in thin sections. It is also generally known that the refining effect of superheating is lost if the melt is held for some time at lower temperatures before casting. Aside from these very qualitative statements, there is little to be found in the literature as to the effect of temperature and time of superheat on the final grain size. Because of the uncertainty of these factors, the Office of Production Research and Development of the War Production Board placed a research contract with the University of California, supervised by the War Metallurgy Committee. This research, which was done under the "Restricted" Project NRC-550, is the basis of this paper, which has been released for publication by the O.P.R.D. The material studied was an alloy prepared from carbothermic magnesium. The temperatures required for grain refinement proved to be widely different from those used in practice, as described in the statements in the first paragraph. This difference is attributed to the fact that the magnesium in the specimens was of carbothermic origin instead of the electrolytic magnesium in common use. Materials and Methods The magnesium alloy studied was one of the most popular sand-casting alloys, with a nominal composition of 9 Per cent aluminum, 2 per cent zinc, and 0.1 per cent (minimum) manganese and the balance magnesium. This is designated

Jan 1, 1945

By D. A. Stevenson, T. Alden, J. Wulff

A portion of the liquidus curve has been determined for the binary alloy systems Ni-Pb and Cr-Pb. The solubility of nickel is 0.53 atomic pet at 372° and 18.63 atomic pet at 1200°C. Chromium shows low solubility, 0.634 atomic pet at 1210°C. Molybdenum and tungsten were also studied and found insoluble in lead, less than 0.005 atomic pet at 1200°C. INCREASED use of liquid metals of low melting X point for heat transfer, coating, joining, and other purposes has renewed interest in the solubility of structural metals in these liquids. A study of Hansen1 and current literature indicates that few liquidus curves at the low melting end of the binary diagrams have been accurately delineated. This statement applies particularly to the binaries of lead. The present paper is limited to nickel, chromium, tungsten, and molybdenum in lead. In early studies2, 3 of the lead end of the Pb-Ni system, a monotectic at 1340°C was established. Tammann and Oelsen' determined the solid solubility of nickel in lead at 20°C to be 0.023 wt pet. Recently Pelzel5 determined the liquidus curve from the eutectic temperature of 327° up to 727°C using a segregation method. In the present paper this part of the curve has been checked and extended to 1244°C. The Pb-Cr system was first studied by Hindrichs.6 He pointed out the existence of a monotectic at 1470°C and indicated a tentative liquidus. Recent corrosion studies of Fe-Cr alloys in lead suggest that chromium is more soluble than iron in lead.7-8 The solubility of tungsten in lead according to Inouye8 is about 30 wt pet at 1200°C. Appreciable solubility of molybdenum in lead might therefore be expected. Experimental Various experimental techniques have been employed in the determination of solubility in liquid metals. For low solubility, thermal analysis is unsatisfactory. A segregation method was used by Pelzel3 in his study of the Pb-Ni system. In this procedure separation of liquid and solid is possible due to difference in density. In the technique of Kleppa10 a single piece of material is maintained in contact with the liquid metal in evacuated Vycor vials. After equilibration, solid and liquid are separated by tilting. Keck and Broder" measured the weight of a piece of the solid solute before and after immersion in a pure solvent bath; the weight loss was a measure of the solubility. All of the above procedures are time-consuming since they permit only one determination per run. Numerous samples for analysis may be taken from the melt in the method described by Gurinsky and CO-workers.10 The rate of extraction of samples is limited only by the time required for equilibration. In the present work, a modification of this method was employed. A 150-g charge of analytical reagent grade lead and the added metal* were contained in an Alun- dum crucible. It rested on firiely divided silica at the closed end of a 45 mm Vycor tube, 500 mm long. The top of the tube was provided with an inlet and

Jan 1, 1959

By E. E. Thurlow

The Geology Div. of Northern Pacific Railway Co. has adapted to its exploration efforts field procedures for geochemical sampling and semi-quantitative analysis which have been developed through research by the U. S. Geological Survey. The sampling is done in conjunction with reconnaissance geologic mapping on aerial photographs or during field checking of maps which have been prepared largely by photo-geologic interpretation. Stream sediment or soil samples are taken and readily soluble combined heavy metals are extracted with ammonium citrate followed by colorimetric titration with dithizone at the sample site. The effectiveness of this approach has been demonstrated both in positive and negative results, thereby assisting in the elimination of large areas of land from further immediate attention and in providing targets for followup exploration. An occa sional sample is submitted for spectrographic analysis as a check on the possible presence of other elements of economic significance. Field laboratory procedures are also being implemented for determining molybdenum, mercury, and other metals which may be valuable in themselves or useful as pathfinder elements in outlining mineralized areas. A lead-zinc occurrence in Oregon and a copper deposit in Montana were readily detected and outlined by stream sediment and soil sampling and a heavy metal anomaly that lacks obvious interpretation has been found in northwestern Montana. Detailed mapping and additional sampling are followed by other exploration techniques if warranted. Northern Pacific's program of reconnaissance mineral evaluation of company-owned lands and adjoining areas was outlined in a paper presented at the American Mining Congress meeting in Las Vegas four years ago. That report included policies and procedures with respect to mineral development on Railway Co. lands and may be referred to for information on these matters.1 In a sense this paper is a progress report on the use of geochemical prospecting in Northern Pacific's continuing mineral evaluation program. At this time there are positive results but as yet there is no real success story in the form of a minable ore body. GEOCHEMICAL PROSPECTING PROCEDURES The decision to use geochemistry as a reconnaissance exploration tool must be followed by research into sampling and analytical methods and into the interpretation of results. Various analytical methods were tried and evaluated by the Geology Div., including hot and cold acid extraction with and without fusion of the sample, panning and magnetic separation followed by dithizone testing of the magnetite, and cold aqueous extraction of metallic ions followed by indicator tests. Samples were first sent to the laboratory for analysis; later field laboratories were established and now virtually all testing is done at the sample site. It was concluded that, where applicable, the quickest dependable methods for reconnaissance use are the dithizone field tests for readily extractable heavy metals. This involves the simultaneous treatment of a sample, usually of soil or stream sediment, with two immiscible liquids; one a cold aqueous extractant (ammonium citrate) and the other a solution of dithizone in toluene or xylene.2 Dithizone is a colorimetric indicator that reacts quantitatively with copper, lead, zinc, and several other metals to form colored complexes in organic solvents. Results may be expressed in ml of 0.001 pct dithizone that are required to reach the blue end point, or calibration of the test results can be carried out with standard solutions of zinc; conversion factors would then be expressed in ppm, zinc equivalent. Calibration of dithizone solution with zinc standards indicates that 1 ml of 0.001 pct dithizone is equivalent to approximately 0.25 ppm of zinc. An authoritative report on dithizone field tests authored by H. E. Hawkes in the June-July 1963 issue of Economic Geology* states "The appeal of these techniques has been the simplicity and speed of the determinations as compared with more tedious laboratory determinations of trace metals in weathered rocks, soils, or plant materials. This obvious appeal, however, has often been more than matched by misuse of the method in such a manner that the results are

Jan 1, 1964

By K. T. Aust

The relative interfacial energies of symmetrical tilt boundaries in silver of greater than 99.999 pct purity were measured as a function of orientation difference 0 between 9° and 36° about <001>. The results are in good agreement with the dislocation model of the grain boundary. The energy vs H curve may be represented by the Shockley and Read equation in the form Eoe (0.55—In 8). READ&apos; has indicated that an ideal experimental method of testing the predictions of the dislocation theory of the grain boundary would be to measure the interfacial energies of symmetrical tilt boundaries between face-centered-cubic grains that have a common <001> axis, as a function of orientation difference 0. The misfit H should be defined by a rotation of each grain through an angle of H/2 away from the boundary. Such boundaries might be expected, from geometrical considerations, to be made up of a series of edge dislocations, at least for small values of 0. Energy vs H relationships for tin&apos; and lead:&apos; were previously obtained for an asymmetrical tilt boundary separating two grains in which generally only one grain was rotated about a <001> specimen axis through an angle of H away from the boundary, the other grain remaining fixed. It is possible, however, that the boundary atoms in tin and lead may have attained a symmetrical position, in relation to the orientations of the grains on either side of the boundary, during equilibrium annealing. The two sets of measurements on silicon ferrite&apos; were somewhat better suited for comparison with theory, since the boundaries were symmetrical tilt boundaries in which the axis of relative rotation was <110> in the first series and <l00> in the second; but this alloy has a body-centered-cubic structure. Although the grain boundaries in silver" were symmetrically tilted, the axis of relative rotation was not a simple crystallographic direction, and it varied from boundary to boundary. Although the above measurements were in good agreement with the Shockley and Read equation,"&apos;: it appeared desirable to carry out experiments under the ideal conditions specified by Read.&apos; Consequently, the relative energies of symmetrical tilt boundaries in silver between grains that have a common <001> axis were measured. The technique of equilibrating grain boundaries in oriented tricrystals was used rather than the less satisfactory thermal groove method previously employed for silver bicrystals." Experimental Details and Observations The solidification and seeding techniques, described previouslyh for growing tricrystals of controlled orientations, were used to prepare tricrystal specimens from silver of greater than 99.999 pct purity. The silver was obtained from American Platinum Works, Newark, N. J., in the form of poly crystalline rods 10 cm long and 7 mm in diam. These rods were then cold worked by rolling or drawing them into suitably shaped blanks. Single crystal seeds and tricrystals were grown in a high purity graphite boat by means of a movable furnace with globar heating elements. The graphite boat was enclosed in a Vycor tube, which was first evacuated to about l00/u Hg and then filled with a static argon atmosphere. The maximum temperature outside the Vycor tube was 1250°C. A typical tricrystal specimen of silver is shown in Fig. 1. Grains B and C were grown from seed crystals with a <001> specimen axis or longitudinal direction parallel to the direction of growth and with another <001> direction perpendicular to the surface. Each of the two seed crystals was rotated 18" about the <001> specimen axis but in opposite directions away from the boundary. A symmetrical tilt boundary, therefore, separated grains B and C with an orientation difference 8 of 36" about <001>. Grain A in Fig. 1 was grown from the middle seed with a <110> direction parallel to the specimen axis and with a <001> direction inclined at 45&apos; to the surface of the specimen. The interfaces sepa-

Jan 1, 1957

A GREAT labor, surely, is that of the coppersmith, since his every work must be hewn from the mass of copper by force of the hammer. At the beginning, middle, and, end all his works are inconvenient pieces and unpleasant to handle. If the work is done on the forge with the fire, it is done in order to refine or compose it into masses again, for drawing these out while hot with the blows of some heavy hammer, or in order to put the works in a condition that allows them to be drawn out while cold and worked. In this he puts all his labor and industry. He who works at this art often makes use of large hammers, sometimes of small ones, and sometimes of those that have a long iron head and a short handle. With these he is obliged ever to proceed in one of these activities, either extending the work lengthwise, narrowing it, or widening it. This is achieved by the manner and direction of striking and therefore it is sometimes hammered on the inside, sometimes on the outside, sometimes with the peen, and sometimes with the flat head. For instance, when he wishes to close it up he strikes it on the outside with the peen, and if he wishes to widen it he strikes it on the inside with either the flat head or the peen. In this way he proceeds to shape it with constant patience, and to make all the vessels that he works graceful. This metal, as I have told you, is soft, flexible, and tenacious under the hammer. It yields with a certain toughness, provided, however, that it is fine and without admixture of a trace of tin or other metal. That craftsman is a good master of this art who best makes every desired work

Jan 1, 1942

A. 0. ASHMAN, Palmerton, Pa. (written discussion *.).-Mr. Newcomb&apos;s paper has interested me greatly, as I have had numerous experiences along this line. I do not think enough emphasis can be put on his warn-ing to keep platinum couples free from contact with quartz tubes, as silica shows a tendency to alloy with platinum to a surprising degree even at low temperatures. I have frequently had evidence of silica contamination in a perfectly good tube, in which there was seemingly no possibility of a reducing atmosphere. This is rather important as it seems to be common practice to insulate, as well as protect, the wires by means of- capillary silica tubing, thus allowing the entire wire to be in contact with the silica. The best way to mount a couple in a silica protecting tube is by means of double-bore porcelain insulating tubes, the protecting tube being slightly longer than the couple so as to leave a space between the couple and the end of the tube. In this way there is no possibility of contamination from silica. In no case should silica capillary tubes be used to insulate platinum wires. Mr. Newcomb states that there is still much to be desired in pyro-meter protecting tubes; this is in keeping with my experience. From a practical standpoint there is not a satisfactory pyrometer tube on the market for high temperatures; with all clue respect to the many improve-ments and good work recently done in this line. I believe that the whole future development of pyrometry is dependent on the development of suitable refractories. With suitable refractories, for example, Darling&apos;s1 work with liquid couples could be developed to a practical basis, making possible the use of base-metal couples to replace platinum.

Jan 12, 1919

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By Otto F. Pfordte

The great advance of the last twenty years in the specialization, delicacy and efficiency of ore-concentrating apparatus calls for a finer system of testing both the qualities of ores and the operations of machines in this department. In amalgamation, lixiviation and smelting, the daily employment of physical and chemical tests has been recognized as necessary, and the cost of the necessary laboratories and employees is cheerfully paid. But while much progress has been made in concentration (due, in a large degree, to the study of the subject in our technical schools), it is still too common in actual practice to follow the loose old method of roughly estimating, once for all, that a given ore " concentrates x tons into one," and resting on this assumption so long as that ore continues to be treated, while assays of the tailings from concentration are made from time to time, without exact determination of their quantity. The first step toward accuracy of control must be a more frequent and precise measurement of the quantity of concentrates from a given operation. This should be expressed in pounds per unit of one ton; and the variations shown in frequent determinations will furnish a constant check upon the character of the ore and the performance of the apparatus. But this is only a part of what should be constantly and systematically done to insure the best work upon a material which must vary continually, even though it come from one mine only. If, in any mill, appropriate laboratory-tests were made at least once a week, the labor and expense involved would be amply repaid by increased knowledge and control of the current operations. A small testing-laboratory, provided with a few gold-pans;

Jan 1, 1902

By Roberto Fernandez

Want of knowledge on the part of experts from abroad respecting the amalgamation-system, known as the Mexican or patio process, has been the cause in this country of trouble to many foreign mining companies. This process has not been looked upon by their managers as a satisfactory method of treating silver-ores, and they prefer to employ others, which, although more modern, and often more profitable in other countries, have not proved to be so under the exceptional conditions of this country, where labor is cheap and paid in silver, while fuel is very dear. The cause of this error of judgment is probably the inexact information which has been furnished by several authors respecting the economical results of the patio process. This treatment is not suitable for silver-ores of every kind. Simple sulphides of silver are best adapted to it, and, next to these, the combinations of complex sulphides, viz., pyrargyrite, polybasite, stephanite, proustite, etc. Chlorides, bromides and iodides of silver are considered rebellious ; argentiferous galena, blende, bournonite, as also argentiferous arsenical pyrites of iron and copper, are absolutelg unsuited to this treatment. Experience has proved that high-grade ores do not give as satisfactory results as those of mediurn grades, as, for instance, carrying from 1 to 2 kilos of silver per metrical ton. The patio process, as actually practiced in this district, comprises the following operations: 1. The ore is crushed in a dry state in a roller-mill, reducing it to pea-size, from which uniform samples, and, in consequence, correct assays, can be obtained. 2. It is then thrown into the arrastra, and pulverized with water, so fine that it will pass through an 80-mesh screen.

Jan 1, 1900

W. L. Saunders, New York, N. Y. (communication to the Secretary*):—The Laramie tunnel, though a small one, compares very favorably in the speed of driving with the great Alpine tunnels which have the record so far. I think it safe to say that, taking all things into consideration, the record made at Laramie is the best American record, though it still falls short of the long-tunnel records abroad. In discussing tunnel-records it must always be borne in mind that there are conditions peculiar to each individual tunnel job, so that no comparisons are complete, fair and conclusive. At Laramie there is one point which stands out prominently, and which distinguishes this from any of the recently-built Alpine tunnels, and that is that here we have great progress in an American driven tunnel without the use of a carriage for mounting the drills. At the Arlberg and Loetschberg tunnels, the carriage was an essential condition for progress. All the heading-drills were mounted upon a bar which rested upon a small carriage. This carriage was withdrawn after the drilling and run into the heading after the blast without much disturbance of the drills, and with very little adjustment except that required in jacking the horizontal bar across the tunnel. The carriage was so small in its track-area that it required little mucking to run it in to the face; and as the rock-drills used were heavy machines 38 in. in diameter, progress in setting up and drilling was very much accelerated by the use of the carriage. At the Laramie tunnel hammer-drills were used instead of piston-drills, and here we have an important distinction which

Jan 1, 1913

By J. Handin

Triaxial compression tests with independently applied external confining pressures and internal pore pressures show that the ultimate compressive strengths of representative oil well cements are nearly linear functions of effective pressure — the difference between external and internal pressures on the jacketed cylindrical specimens (to 15,000 psi). The strengths are little affected by the test temperature to 350F (not to be confused with the curing temperature). At an effective pressure of 15,000 psi, strengths are in the rage of 30,000 to 50,000 psi, comparable to those of sedimentary rocks under similar conditions. The cements become very ductile even under low effective pressures; permanent shortenings of 30 per cent or more are attainable without rupture. INTRODUCTION Since the pioneering work of Richart, Brandtzaeg and Brown1 on the failure of cement under combined compressive stresses, it has been recognized that ultimate compressive strength is greatly enhanced by the application of confining pressure. More recently, Mc Henry2 showed that the strength of concrete was a linear function of the effective pressure (the difference between the external confining pressure on a jacketed specimen and the internal fluid pore pressure), at least for a range of 0 to 1,500 psi. The effect of temperature had not been investigated, and no previous systematic triaxial compression testing of naterials used for oilwell cementing seems to have been done. The present work was suggested by the late J. hi. Bugbee3 who stated that "consideration of the common application of high-pressure hydraulic fracturing to the initial completion or recompletion of wells, and the large pressure drawdowns in some producing wells, particularly those in abnormally high-pressure gas-condensate reservoirs, raises the question of what is a suitable cement strength for various completions. The intuitive belief exists that cement strength need be no greater than formation strength. Tests should, however, be conducted at downhole conditions." The ultimate compressive strengths of rocks penetrated by the borehole must rise several fold with increasing depth.4 This marked enhancement of strength is due to the influence of the effective pressure, the total weight per unit area of the overburden less the hydrostatic pore pressure. (The effect of temperature due to the geothermal gradients is relatively small for depths to 30,000 ft.) .A significant comparison of the strengths of rocks and cements at downhole conditions requires knowledge of the confined compressive strengths of cements as well. EXPERIMENTAL PROCEDURES The theory and technique of triaxial compression testing are fully discussed in earlier reports.4-6 Briefly, cylindrical specimens 1-in. long and 0.5-in. in diameter are jacketed in thin copper tubes of negligible strength, placed in the test chamber and subjected to an external confining pressure of kerosene and loaded axially by the piston at a strain rate of 1 per cent per minute. Pore pressures of water (or kerosene) are applied independently through the hollow piston and are maintained constant during the shortening of the specimen, Tests at sensibly 0 pore pressure are arranged so that any free water in the cement can escape to the atmosphere. (If egress of water were denied, pore pressure would rapidly attain the value of the external confining pressure because of reduction of pore space.) The test chamber can be heated for high-temperature experiments. Unless otherwise noted, the cement samples were air dried for about a week. Recorded during a test are pore and confining pressures, shortening and axial differential force (total force less the product of the confining pressure and the area of the piston). True stress-strain curves are constructed by dividing the measured differential force by the actual cross-sectional area of the specimen at a given

Jan 1, 1966

By David R. Mitchell, Byron M. Bird

THE revision of this chapter has presented a problem in that heavy-medium jigging has come into the picture since the chapter was originally written (seven years ago), a practice in which an artificial medium is built up and maintained in the jig circuit. As this development makes the jig a "true" heavy-medium process, the method belongs in the chapter dealing with such processes. Although putting this development in its proper position in the book involves some repetition, this seems to be the best procedure, and it has been followed. As the chapter on jigs in its original form was intended to be more or less a handbook on jigging for the use of the practical man, and the great bulk of the material therein is still generally applicable, the text has been re-used in large measure. Two major changes should be noted: (1) the portion of the text relating to the refuse-withdrawing mechanism of the McNally-Pittsburg jig has been entirely rewritten, and (2) a description of the hutch valves on the Jeffrey jigs has been added. Jigging is the stratification of a mass of solid particles in upward and downward pulsations. The stratification usually is effected in a rectangular open-top container having a perforated bottom through which the pulsations of water are applied to the materials to be separated; in separating coal, to a mass of coal and refuse. Jigging usually is a continuous process involving three steps: (1) the reception of the raw coal, (2) the stratification of the coal and refuse so that the refuse settles to the screen plate, and (3) the overflow of the cleaned coal and the withdrawal of the refuse collected on the screen. The jig is the most universal washer ever devised. It is handling in practice a wide range of closely sized coals and ores, mixed sizes of coal from 8-in. to 0 through 3/4-in. to 0, and mixed sizes of ores down to 7/32-in. to 0and even smaller. It is treating materials ranging in specific gravity from that of gold at 19 to that of coal at 1.30. It is handling feeds in which the proportions of high-gravity materials range from 90 per cent or higher, as for some iron ores, to 10 per cent or less for some coals. It is handling feeds containing all shapes of particles-round, rectangular, and flat. It is handling simple separation problems and difficult separation problems.

Jan 1, 1950

By L. B. Lindemuth

To those who are in a position to carry the thought to a conclusion; I would like to present a theory for the cause of blisters in galvanized sheets. Blisters that are caused from piping and shrinkage cavities will not be considered because the reason for their formation is entirely obvious. Blisters that occur periodically with no apparent system of ocation, number, size or grouping, and then disappear with no. apparent change in manufacturing method, are the ones to which this theory would apply. Examination of blisters of the latter type has shown that they contain hydrogen gas at atmospheric pressure, and that occasionally traces of oxide or sulfide are found on the inner surface of the blisters. These two characteristics have led to the rather general idea that hydrogen gas generated in pickling, and that iron oxide supposed to be inherent in the ingot and causing weak spots were, in some manner, responsible for the development of blisters in galvanizing. The theory which I wish to advance is that these blisters are caused by moisture that has penetrated the steel after the annealing operation. This moisture comes from the atmosphere, or from pickling or washing and when it is suddenly expanded into superheated steam in galvanizing, the increase in volume is so great that it cannot escape with sufficient rapidity through the small opening where it entered as moisture.The pressure so generated forces the sheet apart along those lines of lamination ;hat may be found in practically all flat sections of steel rolled comparatively cold. The increase in volume. from moisture to steam at 800° F. is 2244 times the original volume of the moisture. The pressure generated by ;he moisture heated to 800° F. and entirely confined would be enough to expand or explode any container. This would explain the source of sufficient pressure to cause a sheet to blister.

Jan 3, 1927

By Albert R. Ledoux

I am indebted to The Kaolin Co. of West Cornwall, Conn., and particularly to its engineer, Mr. M. Wanner, for permission to make public, through the Transactions of the American Institute of Mining Engineers, the interesting results of his experiments, having in view the winning of kaolin from deep deposits without shaft-sinking or removing of the overburden. So far as I am aware, nothing like it has been accomplished heretofore, although it reminds one of the methods successfully employed in Louisiana for the winning of sulphur from deep beds by the sinking of pipes one within another, injecting superheated steam under pressure through one pipe, the heat of the steam liquefying the sulphur and the pressure forcing it up through the other pipe to bins at the surface. The kaolin-deposit at West Cornwall is an alteration in situ— that is, it is not sedimentary. A series of clay-veins, dipping about 50" from the vertical, lie between a foot-wall of&apos; limonite and a hanging-wall of gneiss and hornblende schist. The clay-veins alternate with veins or seams of more or less broken quartz, and unaltered feldspar. The deposit, which occurs at a point about 600 ft. above the Housatonic river, was opened five years ago, and about 5,000 tons of a superior grade of washed kaolin have been extracted from open pits, and sold. It soon became evident that this mode of extracting the product would prove unremunerative, by reason of the dip of the vein and the intercalary strata and lenses of quartz, and a more satisfactory method of working the deposit was sought. It is well understood that, in the preparation of all clays for market, especially residuary kaolin, the most important as well as the most difficult step is the washing of the crude product. The dificulties increaee with the percentage of foreign matter, especially quartz and mica, contained in the product. Hence, a system

Jan 1, 1907

By Walter O. Snelling

In combating mine-fires the use of carbon dioxide as a means of producing an atmosphere in which combustion cannot be sustained, has been many times suggested and frequently tried, generally with a fair degree of success. The carbon dioxide is produced by acting on limestone with dilute sulphuric acid, large wooden boxes being used to hold the limestone, and arranged in such a manner that one box may be cleaned and refilled with blocks of limestone while another is being used in generating the carbon dioxide.. The gas is led by means of pipes of large diameter to the location of the fire, tight brattices having been previously put up as close to the fire as possible on every side, so as to limit the space to be filled with the gas to the smallest possible volume. The cost of producing carbon dioxide has been, however, a decided draw-hack to the use of this method, and the danger of producing carbon monoxide by the reduction of the carbon dioxide by heated carbon, and consequently bringing about an explosion, has also tended to prevent the application of this method. The use of sulphur dioxide in combating mine-fires has not, I believe, been previously suggested or tried, and yet the method presents such decided advantages over the use of carbon dioxide that it seems proper to suggest the advisability of considering it as a cheap, convenient, and safe means of fightr ing stubborn mine-fires. 1. Cost, Preparation, etc.—One ton of brimstone, costing from $20 to $30, will produce about 25,000 cu. ft. of sulphur dioxide gas, and allowing for all sources of loss it is probable that sulphur dioxide gas can be produced for about $1,300 per 1,000,000 cu. ft. For carbon dioxide gas, produced by the action of sulphuric acid on limestone, a good estimate would be $4,000 per 1,000,000 cu. ft., provided that sulphuric acid

Jan 1, 1909