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By C. M. Romanowitz, H. A. Sawin

PLACER dredging as we know it today, especially gold dredging, is an industry about 40 years old, dating from the beginning of this century, when a few mining men in California saw the possibilities in adapting earlier dredging methods to California placer fields in and immediately adjacent to streams. At first it was thought that dredges must be operated in existing stream beds, but experience soon pointed the way to dredging alluvial deposits of old stream beds, operating on landlocked dredging ponds. Within the first five or six years of modern dredging, experience was gained so rapidly that dredges to dig 60 ft. below water level were designed and built. This depth was believed by many operators to be the maximum at which successful dredging could be carried on. Alluvial deposits of gold, suitable for dredging, were readily handled by equipment available and developed early in the industry's history. Much of the gravel was easily dug and if deposits were cemented, contained large boulders, or for some other reason could not be handled by a dredge, the ground was abandoned in favor of other deposits that could be handled easily. Many failures, adversely affecting the dredging industry, resulted from attempts at that time to extend the scope of placer dredging with equipment not suited to the formation being dredged. Dredging ground suited to early equipment was exhausted eventually, but many supposedly undredgeable alluvial fields containing gold in commercial quantities were found and became known to dredgemen. Improved equipment was needed to work deposits known to exist at great depths or associated with unusual obstructions. Operating companies looked to dredge manufacturers and metallurgists, particularly manganese-steel foundries, for improved designs and materials. Experience developed in California has spread throughout the world, and dredges of improved types have been adapted to the mining of platinum and tin as well as gold. Space will not permit a description of all the improvements in dredging since the early days, but a few of the recent developments are worthy of note, because they make possible the dredging of placer deposits of great depth, those having hard, irregular bedrock or containing large boulders in great quantities, and compacted or cemented gravel deposits. DEEP DREDGING At Hammonton, Calif., Yuba Consolidated Gold Fields has, within the past two years, built its dredge No. 20. The company has operated continuously in that field since 1904, digging successively at maximum depths of 60 ft., 8o ft., 112 ft., and now 124 ft. below water level. The first dredges were equipped with buckets of 6 and 7 ½ -cu- ft. capacity; six dredges operating in the field today have 18-cu. ft. buckets, digging now 65 to 124 ft. below water level. Some ground near Hammonton has been dug for the third time, owing to the devel-

Jan 1, 1941

By H. R. Reed

THE cost of hoisting with electricity in deep mines is a matter about which little information has been published. This paper makes a detailed study of such costs and presents the information in a series of curves. In particular the curves show the cost of hoisting ore from depths varying from 500 to 7000 ft. Vertical with the shaft at 70° incline for the double cylindroconical and double cylindrical drums, the hoists operating balanced, using Ward Leonard and Ilgner-Ward Leonard control, and designed for most economical operation from each depth. Operation with the double cylindrical drum is expanded to cover hoisting from 2000 to 5000 ft. using equipment designed for 5000 ft. and from 4000 to 7000 ft. using equipment designed for, 7000 ft. Additional curves are included to show the ratings of the necessary hoist motors, energy input per hoisting cycle and size of flywheel in tons for complete equalization when the Ilgner-Ward Leonard system is used, also hoisting efficiency. The duty imposed on a mine-hoist motor fluctuates between wide limits during a cycle of operation. The demand on the motor may vary from a large horsepower value' near the beginning of the cycle to a small or a negative demand near the end of the cycle. Such factors as tonnage to be raised per hour, depth of shaft, and balanced or unbalanced opera-tion have such a marked effect on the operating cycle and vary to such an extent for different mines that no set of rules can he formulated for quickly determining the size of the motor required. The duty cycle from which the motor rating is (derived must he determined for each case according to the conditions of the proposed hoisting operations. The motor torque required at the cardinal points of the duty cycle is determined from the moment or torque in pound-feet necessary to raise and lower the load and ropes, accelerate and retard the load, ropes, drum, etc. The torque diagram depends largely upon the type of drum. Two different types of drums, if used on exactly the same duty cycles, may have widely different peak demands and capacities of hoist motors. The essential feature in the design of hoisting drums and in determining

Jan 1, 1937

By W. O. Philbrook, K. M. Goldman, G. Derge

EQUILIBRIUM conditions for steelmaking reactions have been studied extensively over the past two decades by a .number of investigators, with gratifying results. Equilibrium data are essential to the understanding of any process, and such knowledge has the practical utility of placing a limit beyond which control measures cannot succeed. When, however, the driving rate of an industrial process is so fast that there is not time for reactions to reach equilibrium, it then becomes necessary that the factors which control the rates of reaction be known in order to establish full control of the process. The desulphurization of molten pig iron by slags within the iron blast furnace is one such process in which the actual degree of sulphur absorption by the slag does not approach the equilibrium distribution obtained for similar slag-metal systems in the laboratory.' A study of the rate-controlling factors governing the desulphurization of iron by slags is becoming increasingly important as the sulphur content of raw materials increases with depletion of higher grade ores and coal. Following up an initial study on kinetics,' this paper reports some results of a continuing laboratory investigation on the mechanism of sulphur transfer between molten iron saturated with carbon and slags of the CaO-SiO,-A12O3 system. Laboratory experiments cannot reproduce in detail the conditions which prevail in the hearth of a blast furnace, but they will contribute to an understanding of the smelting reactions and perhaps will explain some apparent inconsistencies in the factors controlling the equilibrium distribution of sulphur between iron and slags under reducing compared with oxidizing conditions. The mechanism of a reaction—that is, the individual steps and the sequence in which they occur to produce the overall reaction which is ordinarily observed—must be elucidated to learn which steps are the slow ones, or "bottlenecks," that fix the pace of the process as a whole. In the desulphurization reaction, for example, the overall rate might, in principle, depend upon the rate of diffusion of sulphur in the metal or in the slag, upon the speed of some homogeneous reaction taking place entirely within one of the phases, or upon some heterogeneous reaction taking place across the slag-metal interface. Even some side reaction or the back reaction might have some influence. Evidence on all of these points will be presented in this paper. The rate of diffusion of sulphur in both iron and slag is so slow that it seems necessary to assume that convection provides the mechanism of carrying

Jan 1, 1951

By Adrian C. Dorenfeld

Laboratory data form the basis for the design of flotation circuits. These data, obtained from testing samples of the ore, should show the optimum con- ditions for concentrating the ore and the effects of change in process vari- ables. Among the more important variables commonly met in flotation practice are: Liberation Size-This is the particle size at which substantially all of the valuable minerals are detached from the gangue minerals. Reagent Additions- Experimental data will show the reagents used and their quantity, quality, and point of addition. Pulp Density-This is an important variable in the design of the flotation circuit because it is one of the factors determining the size and number of flotation cells. Flotation Time-The time necessary to make the separation into concentrate and tailing depends on such factors as particle size and reagents used and must be known for determination of the size and number of flotation cells in the plant. Temperature of Pulp-Temperature affects flotation reactions. Water at approximately room temperature is satisfactory for most flotation separations, but some minerals such as fluorspar are best floated in hot water. Type of Circuit-Many types of circuits can be designed, as discussed in detail later. The laboratory tests should provide data for design of the plant circuit best suited to the ore. Water-Knowledge of the quality of the future plant's raw water is important because water quality may drastically affect flotation results. If possible, flotation tests should be made using samples of the water to be used in the plant. Flotation results may vary with seasonal temperatures and with circulation of reclaimed water. Experimentation can show whether it will be necessary to provide for heating, cooling, treating, or reclaiming the water. Uniformity of Ore-The extent of variation of the ore in hardness, grind- ability, mineral content, and floatability should be investigated so that the designer can ascertain methods to overcome problems caused by ore variations. Settling and Filtration Data-To design the plant flotation circuits, settling and filtration rates and ultimate percentage solids of the various products must be determined. Corrosion and Erosion-Corrosion and erosion tests should be made on the flotation pulps, particularly if the pulps are acid or at an elevated temperature, so that suitable materials of construction can then be chosen.

Jan 1, 1962

F. AT. FARMER*, New York (written discussion?)- The paper presents many phases of the welding art concerning which there are very divergent views. In many cases, the wide differences of opinion are based on the results of mechanical tests, but an examination of the mechanical test data discloses a wide variation in character of the tests made and in the details of procedure, so that it is frequently not only difficult to analyze and check the basis of the conclusions but impossible to correlate various groups of test results. It would seem, therefore, that the technique of testing welds is one of the phases of the welding art that should be studied and standardized in order that the results of mechanical tests made by different people may be strictly comparable and have the same significance to all. The vital difference between testing a specimen of steel that includes a welded joint and testing an ordinary specimen is the non-homogeneity of the weld specimen. The weld specimen has at its center a section composed of material that usually has physical, chemical, and metallurgical characteristics distinctly different from the adjoining metal. Furthermore, the section of added metal is more or less irregular and the ratio of added metal to original metal in the section is quite variable. Consequently the details of procedure and of recording data should be more minutely prescribed than in the testing of ordinary specimens. A conspicuous example f a mechanical test that requires standardization is the cold bending test, a standard test for mild steel. With the usual method, the specimen is bent around. a pin of prescribed diameter and, as all specifications usually require bending to 180° without fracture, the manner of applying the load is immaterial because the specimen is ultimately completely wrapped around the pin. But a specimen containing a welded joint at the center will usually not withstand bending to 180° because of the much lower ductility of the deposited metal in the weld. It is therefore obvious that the farther apart the points of support are the greater will be the angle attained before cracking occurs, simply because most of the bending will take place in the original metal. It is therefore highly desirable that there be prescribed a standard test that fixes exactly the distance between the supports, the curvature of the surface of supports, and the relation between this curvature, that of the loading surface, and the thickness of the specimen.

Jan 5, 1919

By E. J. Rapperport, J. P. Pemsler

The thermodynamic activities of zinc in six solid solution Cu-Zn alloys ranging from 5 to 35 at. pct Zn were determined experimentally in the temperature range 400° to 600°C. This low temperature investigation was canducted in order to evaluate techniques developed to utilize the inherently high sensitivity of atomic absorption flocesses in the measurement of thermodynamic activities. Analytical expressions ,for the activity and actizlity coeflcient are given for the six alloys in the temperature ranges investigated. RELATIVELY few experimental methods are available for investigation of thermodynamic activities of alloys, especially in the solid state. The techniques most frequently used have been the electrochemical potential and the effusion methods, both of which have severe limitations in many instances. It is therefore desirable to expand the ability to perform such measurements in order to obtain new information as well as to provide an additional independent verification capability. In this work, we present a significant improvement in the spectrophotometric method for sensing small vapor pressures in static absorption cells. Similar techniques have been used previously;1"5 however, applications had been limited to relatively high pressures, often greater than 1 torr. Prior investigators have, for the most part, used broad spectral sources such as xenon or mercury lamps, and high intensity arcs. Hollow cathode sources were first suggested in 1956 6 and were used soon afterwards.4'5 These sources offer significant improvements in sensitivity and freedom from interfering spectral lines.'-' EXPERIMENTAL High purity zinc was obtained from Cominco Products, Inc., and copper from American Smelting and Refining Co. Both elements were of 99.999 pct purity. Copper-zinc alloys were vacuum melted in a high fired carbon crucible with each alloy pulled from the melt as a 4 -in. diam bar. The bars were swaged to -1/4 in. rods and vacuum annealed for 160 hr at 800° + 1°C. Samples for gross chemical analysis were taken at intervals along the length of the rods to ascertain the axial zinc gradient. Electron microprobe analysis of homogenized specimens indicated that the alloys had uniform compositions over their cross sections on a macro (200 p) and micro (1 u) scale to better than *1 pct (20) of the gross composition. This tolerance was determined by counting statistics, rather than assured composition fluctuations. All SiO 2 windows were high-ultraviolet-transmission grade to minimize intensity losses. Silica absorption cells were scrupulously cleaned consecutively in organic solvents, dilute HF, and distilled water before use. The empty cells were then flamed while under a dynamic vacuum, cooled, and removed to an argon-filled glove bag. Alloy pieces were cut and filed in the glove bag to produce fresh surfaces, and then loaded into the cells. The loaded cells were temporarily sealed, removed from the glove bag, reevacuated to 10-5 torr or better, and permanently sealed. The instrument used is schematically shown in Fig. 1. The spectral emission from a commercially made hollow cathode lamp (A) of a selected element is focused through an absorption cell (B) inside a well-controlled furnace (C). The intensity of the transmitted beam is measured using the spectrometer* (D) 'Techtron model AA4 atomic absorption spectrometer. which contains a grating (E) that disperses the light prior to impingement on the photomultiplier (F). The monochromator grating is adjusted so that only the wavelength of interest is measured. The power supply delivered an interrupted voltage to the lamp, causing a chopped radiation output to be transmitted. The detector read only the intermittent component of radiation incident upon it, so that all continuous noise signals (furnace radiation, and so forth) were eliminated. Three recording thermocouples contained in the muffle furnace were positioned along the length of the absorption cell: one at each end and one at the center. An effort was made to keep the ends of the cell several degrees hotter than the center to avoid window condensate. Appropriate thermal corrections were then necessary to relate cell pressure to radiation attenuation. Water-cooled heat shields, as shown in Fig. 1, were found to aid signal stability by protecting the hollow cathode and the photomultiplier from furnace radiation. The furnace had a 2-in. diam muffle, Kan-thal wound, with SiO 2 windows at its ends to minimize convective effects. The hollow cathode radiation was masked and focused to form a conic beam that was a maximum of { in. diam within the furnace. Thus, the 1.5 in. diam absorption cell easily contained the entire beam. The furnace was mounted on ball-bearing slides with positive positioning detents. This arrangement allowed the removal of the entire furnace assembly from the radiation path, position [I], Fig. 1, so that frequent sampling of the unattenuated beam intensity could be obtained. In all cases the beam intensity was kept constant to 0.1 pct as judged by readings taken immediately before and immediately after data collection. Only data for absorptions of less than 80 pct were utilized, as systematic deviations from linearity were found for greater absorptions.

Jan 1, 1970

By Albert H. Fay, William B. Plank

In practically all rock-excavation problem there is need for a careful study of the rock structure, its fault, cleavage or bedding planes, and even the texture of the rock itself. These studies should form the bases upon which an excavation method is selected and they should be carefully considered in predicting the amount and extent of the excavation. The need for such studies was forcibly illustrated in the problems involved in a cut made in 1929, along and underneath a 200-ft. high rock projection for a State highway near the City of Easton, Pennsylvania. The rock mass was badly faulted and also contained a number of cleavage planes at approximately right angles to the fault planes. Much of this structure was visible and could have been studied and analyzed before the work was begun. The State had rigid specifications as to finished grade and slope of cut, which apparently were made without reference to the geologic structure. The contractor complied with the specifications, under the close inspection of the State engineers. A tunnel blast was placed in the base of the cliff, with the result that 65 per cent more rock was broken than was intended by the specifications. About four years after the blast, the writers of this paper studied the circumstances surrounding the operation, to determine the cause of this excess excavation. Scope of Work The section of the roadway involved was about 200 ft. long and on a 6' curve. It was necessary to relocate points on the curve, from which all faults and cleavage planes were located and measured by the use of transit and clinometer. A plan (Fig. 1) showing the blasting tunnel, the roadway, and traces of the faults and cleavage planes on the level of the roadway, was prepared; also 13 cross-sections at varying intervals, showing the original face of the hill and the face after the blast. The original and final profiles of the rock face, taken from the plans of the State engineers, are shown in Figs. 2, 3 and 4.

Jan 1, 1937

By K. W. Smith, E. A. Thomas

Various grades of synthetic mullite have been developed in recent years to replace or supplement natural sources of mullite deriued from the mullite group of minerals consisting of sillimanite, kyanite, and andalusite. Raw materials and heat treating processes used in making synthetic mullite are described. Chemical and physical data are given for typical grades and crystalline structure is illustrated with micrographs. Use of synthetic mullite as a refractory material in the glass and metallurgical industries is discussed. Mullite (3A12O3.2siO2), the only stable compound formed in the alumina-silica system, is usually present to some degree in all aluminum silicate ceramic products. The formation of mullite is considered beneficial to give rigidity to the structure and is dependent upon the ratio of Al2O3 to SiO2 in the original composition, particle size, degree of mixing, firing temperature, cooling rate, and the presence of auxiliary glass-forming fluxes. Mullite may also be formed at the reaction interface of fire clay or alumina-type refractories in contact with glass or slag melts. The term synthetic mullite is commonly used today to identify a class of sintered and fused aggregates or grains in the alumina-silica system having a highly developed mullite structure but derived mainly from raw materials other than the sillimanite group of minerals. Within the past 15 years extensive research has been done to develop economical processes to form sintered synthetic mullite aggregate to replace calcined Indian kyanite in super-refractories. Severa1 brands of such mullite are now being produced in commerical quantity and finding extensive use in refractories. Based on the service results of such refractories in many applications throughout the metallurgical, ceramic, and glass industry these developments have been considered successful and suitable substitutes for Indian kyanite now appear assured. EARLY DEVELOPMENT The conversion of kyanite, sillimanite and anda-lusite minerals of the sillimanite group to mullite and their use in refractories and porcelain have been discussed quite extensively in the literature by peck,' Grieg,' Riddle and Foster,3 Bowen and Grieg,4 and others and will only be mentioned here for reference to compare properties with synthetic mullite. In 1928, curtis5 reported on the development of a high temperature gas-converter process for forming synthetic mullite. The raw materials were derived mainly from lumps of high alumina clay of the correct natural composition or blends of clays and alumina that was interground and briquetted to form a suitable charge to maintain a surface combustion firing within the converter. Curtis was, no doubt, the first to illustrate by micrographs in natural color the crystalline structure of mullite derived from kyanite and mullite derived by sintering clay and alumina mixtures at temperatures above cone 32 (3123°F) and by electric fusion. In 1937, sei16 was issued a patent covering the use of a mixture of alumina-silica minerals and alumina in the proportion to form a mullite-yielding material at temperatures in excess of 3100' F. During the period from 1930 to 1940, economic conditions were not favorable for the production of synthetic mullite mainly due to an adequate supply of good grades of Indian kyanite ore suitable for conversion to mullite. Uncertain conditions on availability of the Indian kyanite during the early stages of World War II fostered further study on the development of synthetic substitutes. In 1943, McVay and wilson7 reported on an extensive investigation of domestic substitute materials. Their work covered essentially the use of mixtures of electric furnace mullite, calcined topaz, and calcined domestic kyanite. Compositions were found that gave equivalent or better hot load strength than Indian kyanite in mullite-type brick compositions; however, the calcining of the topaz presented certain physical and chemical problems on the disposition of silicofluoride and hydrofluoric acid while the high cost of electric furnace mullite was a limiting factor. In this work it was pointed out that water-quenched fused mullite was found to be unstable on reheat and gave poor hot load strength due to excessive glass present whereas the slow cooled or annealed mullite contained large crystals of mullite and corundum with little glass and gave superior results.

Jan 1, 1961

By M. E. Wadsworth, W. H. Dresher, W. M. Fassell

HIGH temperature-high pressure techniques have long been used to great advantage in the organic chemical industry, the petroleum industry, and the paper industry. Only recently, however, have these methods been used to extract metals from their ores on a commercial scale. The Chemical Construction Corp., together with interested producers of nickel and cobalt, has done much to develop methods of producing nickel and cobalt powders by the use of high temperature-high pressure techniques.' The Howe Sound Co. is currently operating a plant near Salt Lake City in which the new Chemical Construction Corp. technique is applied to cobalt-arsenic sulfide concentrates. In this method the concentrates are leached in a dilute solution of sulfuric acid under air pressure at a high temperature. Near Edmonton, in Alberta, Canada, the Sherritt Gordon Co. is also using the new method in conjunction with its ammoniacal leach process.' National Lead Co., at Fredricktown, Mo., is operating a process similar to that of Howe Sound. In spite of the rapid growth of high temperature-high pressure hydrometallurgical processes, there has been very little work done on fundamental principles involved in this type of process. Conse- quently the literature lacks any significant data in this field. Oxidation of pyrite,3 sphalerite,4 galena," and recently molybdenite" in alkaline solutions has been reported to some extent. This investigation was initiated, therefore, to broaden the application of high temperature-high pressure hydrometallurgy and also to contribute some insight into the basic mechanisms of oxidation in an aqueous medium under these conditions. In addition to the immediate consequences of these processes much valuable information remains to be learned about fundamental reactions when they are carried out at temperatures and pressures slightly higher than those normally encountered. Leaching of molybdenite by alkaline solutions under oxygen pressure has recently been reported in the Russian literature by E. S. Usataya,6 ho found that leaching rate increased with an increase in the pH of the solution—the strongest effects being observed at a pH of 10—and also with an increase in temperature. Usataya also has reported the formation of a protective film on the surface of the molybdenite when the leaching solution was weakly alkaline, neutral, or acidic. He believes that this oxidation process explains the migration of Mo++ in the oxidation zones of molybdenite ore deposits and the subsequent impoverishment of the ores. Equipment: The high temperature-high pressure reaction unit used in this work was especially designed for kinetic studies of this nature, emphasis being placed on accuracy of measurement and precision of control. As details of the unit's construction and operation have been discussed elsewhere,' only basic features and principles of operation will be discussed at this point.

Jan 1, 1957

By L. D. Lash, J. R. Ross

Discovery of scandium in the Vitro solvent extraction plant for uranium led to commercial recovery of the byproduct. Micro amounts of scandium were extracted with uranium by dodecyl phosphoric acid, but failed to follow ura-niuminto the hydrochloric acid strip solution and were eventually concentrated in the organic extractant. A fluoride strip system was developed to recover scandium from the solvent in concentrated form. High purity scandium oxide was then prepared in multi-pound lots by chemical separation techniques. The plant recovery operation, final product purification, and analytical procedures are described. Scandium is a pseudo-rare earth which is truly rare and expensive. It has special properties which may make it desirable even at the present price of $2750 per lb. Recently the price was lowered from $5000 per Ib which had prevailed since 1952, and it is anticipated that usage will be stimulated because of the lowered price. This metallic element is distributed widely in trace amounts in the rocks of the earth's crust. In addition to micro-amounts found in most uranium ores, concentrations of 50 to 100 ppm have been found in Colorado ferberite ore, lateritic nickel ore, heavy sandstone from Utah, Wyoming, and New Mexico, and various zircon sands and monazites from the western part of the U. S. Scandium has been found as an essential constituent of very few minerals, the most important being thortveitite, a scandium silicate. At the present time, this mineral commands a price more than twice that of gold. Chemically, scandium is in group 3A of the periodic table. It is closely associated with yttrium and the rare earths which it strongly resembles in its reactions. It has a valence of three and will form an insoluble hydroxide, fluoride, or oxalate under proper conditions, similar to the rare earths. Eight years before its discovery, scandium was predicted by Mendeleef who ascribed his eka-boron with properties nearly identical to the actual properties of scandium. Its position as the element with Atomic No. 21 and Atomic Weight 44.96 places it between calcium and titanium in Period 4 of the chart. The successful commercial application of scandium must depend on unique properties to justify use of this high cost substance. Greater consumption would allow additional price reductions, but scan- dium will remain a relatively high-priced commodity because of its inherent scarcity. Research reportedly has been oriented toward use of scandium as an agent to achieve high-temperature, low-density alloys with magnesium and tantalum.' Also, the U.S. Air Force sponsored a project for production of research amounts of pure scandium metal.' The oxide has been used experimentally in electronics, ceramics, and metallurgy. The various aspects of scandium are well covered in recent publications.s-5 CONCENTRATE RECOVERY Small amounts of scandium exist in uranium ores and are dissolved during an acid leach yielding up to 0.001 gpl Sc2O9. When Vitro converted their uranium plant from phosphate precipitation to solvent extraction: scandium was found to follow the uranium into the dodecyl phosphoric acid solvent (DDPA). However, scandium did not strip with uranium from the DDPA in hydrochloric acid, but remained in the solvent. Therefore, a concentration of scandium built up in the organic phase. Residues from the solvent were spectrographed by the U.S. Bureau of Mines and found to contain scandium. As a result of this discovery, provisions were made in the plant for recovery of scandium-bearing concentrates. Solvent extraction of uranium was added to a conventional acid leach process in a typical installation? The ore was crushed and ground, and then leached with dilute sulfuric acid. Addition of an oxidant such as sodium chlorate insured conversion of uranium minerals to a soluble form. At this point, the slurry was chemically reduced by a sulfide, such as sodium hydrosulfide, to remove substances such as ferric iron and molybdenum which were partially extracted by the solvent. The solids-liquid separation was accomplished by a four-stage counter cur rent decantation (CCD) thickener circuit. The uranium was extracted from pregnant liquor with 0.1M DDPA in kerosene and stripped with ION

Jan 1, 1961

by their overdogmatic picture of geology and their resulting drastic oversimplification and idealization of geologic features. I am in hearty disagreement with the recommendation that geophysics should be done by cooperative work between a geologist and a geophysi-cist. That arrangement would be comparable to doing petrography by having a physicist at the microscope and a geologist sitting by his side. The interpretation of the geological significance of geophysical data can be done efficiently only by a physicist who has become also a good geologist or by a geologist who is also a good geophysicist. Less Well-trained Men The rank and file, composing perhaps two-thirds of the personnel of exploratory geophysics, is not, and should not be, composed of highly trained men. The routine, stereotyped character of the work and the impossibility of promotion of more than a few from these lower ranks even under the best circumstances justify companies in filling the bulk of these rank and file positions with men having only a bachelor's degree at the most. There can be a wide range of training for such positions, although certain lines of study are preferred for certain kinds of work, and different employers have different preferences. For work in gravitational and magnetic prospecting, first preference will be for men having geological training and second for men with civil engineering training. In seismic work, men with geological training are preferred by some employers for computers; physicists, electrical engineers and all whose technical education has covered radio circuits are preferred for the other technical positions. Collegiate training in geophysical prospecting brings no preference and by many employers is given a slightly inferior rating. One large company seldom hires men who have just graduated with a major in geophysical prospecting. This prejudice is based on the reasoning that much of what is learned in college is obsolete or obsolescent, that most of the techniques learned in college will have to be unlearned, because different from those used by the employing company, and that in the long run additional courses in basic physics, mathematics and geology are of more value to a man than the courses on geophysical prospecting. DISCUSSION [This discussion refers to the five papers beginning on page 23 and ending on page 74.1 L. W. Blau,* Houston, Texas.—I have had some rather sad experiences with forecasting. For example, I could not foresee 10 years ago my present occupation, and I do not profess to be able to look ahead 10 years and tell anyone what he will be doing then. Referring to the point raised in the discussion, I do not know, for example, what the price of oil will be 10 years from now. If an appreciable number of

Jan 1, 1940

by their overdogmatic picture of geology and their resulting drastic oversimplification and idealization of geologic features. I am in hearty disagreement with the recommendation that geophysics should be done by cooperative work between a geologist and a geophysi-cist. That arrangement would be comparable to doing petrography by having a physicist at the microscope and a geologist sitting by his side. The interpretation of the geological significance of geophysical data can be done efficiently only by a physicist who has become also a good geologist or by a geologist who is also a good geophysicist. Less Well-trained Men The rank and file, composing perhaps two-thirds of the personnel of exploratory geophysics, is not, and should not be, composed of highly trained men. The routine, stereotyped character of the work and the impossibility of promotion of more than a few from these lower ranks even under the best circumstances justify companies in filling the bulk of these rank and file positions with men having only a bachelor's degree at the most. There can be a wide range of training for such positions, although certain lines of study are preferred for certain kinds of work, and different employers have different preferences. For work in gravitational and magnetic prospecting, first preference will be for men having geological training and second for men with civil engineering training. In seismic work, men with geological training are preferred by some employers for computers; physicists, electrical engineers and all whose technical education has covered radio circuits are preferred for the other technical positions. Collegiate training in geophysical prospecting brings no preference and by many employers is given a slightly inferior rating. One large company seldom hires men who have just graduated with a major in geophysical prospecting. This prejudice is based on the reasoning that much of what is learned in college is obsolete or obsolescent, that most of the techniques learned in college will have to be unlearned, because different from those used by the employing company, and that in the long run additional courses in basic physics, mathematics and geology are of more value to a man than the courses on geophysical prospecting. DISCUSSION [This discussion refers to the five papers beginning on page 23 and ending on page 74.1 L. W. Blau,* Houston, Texas.—I have had some rather sad experiences with forecasting. For example, I could not foresee 10 years ago my present occupation, and I do not profess to be able to look ahead 10 years and tell anyone what he will be doing then. Referring to the point raised in the discussion, I do not know, for example, what the price of oil will be 10 years from now. If an appreciable number of

Jan 1, 1940

By H. L. Overton, J. B. Lipson

The concept of sodium single-ion equivalent activity as developed by Gondouin, Tixier and Simard,' was used to determine the filtrate resistivity-activity relationships for 150 laboratory and 49 field drilling muds. With the exception of the native and phosphate high-resistivity muds and the calcium-treated muds, the filtrate resistivity-activity relationships were found to be within 20 per cent of that for pure sodium-chloride solutions. Gondouin, et al,* previously suggested a method of treating the high-resistivity muds in quantitative electrical log analysis. A new treatment is presented which uses the P-alkalinity of the filtrate as a correlating parameter in handling the calcium-treated muds in quantitative electrical log analysis. INTRODUCTION Gondouin, Tixier, and Simard in 1957 introduced new interpretive procedures for analyzing the self-potential curve of electric logging. They re-emphasized the previous work of the Schlumberger brothers, Wyllie and others, and re-defined the activity concept in terms of a number which they termed the effective resistivity. Their procedures are particuarly effective when the connate-water resistivities are less than 0.08 ohm-m or greater than 0.3 ohm-m. For gyp muds where the calcium content is known, a procedure was presented which allows calculation of the connate-water resistivity with improved accuracy. These procedures assume that one of the fluids in the system is a pure sodium-chloride solution, but they are not limited by the assumptions. For the fresh and saline connate waters, for instance, it is assumed that the drilling mud filtrate is a pure sodium-chloride solution. For the gyp mud interpretive procedure, it is assumed that the connate water is a pure sodium-chloride solution. Brown,' on the other hand, has suggested that it would be extremely fortuitous if drilling mud filtrates could all be treated electrochemically as sodium-chloride solutions, and he cites some examples where discrepancies exist. A study has been made of the deviations of sodium single-ion equivalent activities, an of drilling mud filtrates from that of pure sodium-chloride solutions. Drilling fluids in common use on the Texas and Louisiana Gulf Coast and laboratory-controlled muds were investigated. Using a cell patterned after Gondouin, et al, (Fig. I), the equivalent activities were measured. It should be remembered here that the activity measured is merely an index which uses numbers that represent the sodium single-ion equivalent activity a,., of the mud filtrate. The membrane potential developed across the cell was determined with a null-type potentiometer. The resistivities of the solutions were measured by the four-electrode method. The resistivity system was calibrated by using saturated KC1 solution as a standard. Chemical properties of the drilling fluids studied were measured with standard API-approved equipment for the particular property in question. For the activity measurements, two shale discs were chosen to serve as cationic membranes. These two discs were both 1 1/4 in. in diameter and, respectively, 1/4 and 1/8 in. in thickness. The membrane potential, Em, was determined using the shale discs as cationic selective membranes separating two standard sodium-chloride solutions of known mean activity. Then by comparing the constant Km in the following equation, with the theoretical value of — 59 mv at 75OF, the perfection of the membrane was determined. The variation of Km for the two membranes used in this experimental work, as well as one of the many unsuitable membranes, is shown in Fig. 2. The measurement of the activity of mud filtrate involves the balancing of its combined individual activities against a standard solution of known mean activity. At the point where there exists zero potential across the membrane cell, the activity effects may be assumed equal for all practical purposes. The mechanics of making a null reading of this sort requires having a large number of different mean activity solutions. A more practical method involves

By Frederick Prime

THE Great or Cumberland Valley, which (under a variety of names) extends from Canada, through Vermont, Massachusetts, Connecticut, New York, Pennsylvania, Maryland, Virginia, and East Tennessee, to Alabama, is composed in part of limestones lying immediately above the Potsdam sandstone. Geologically, they belong to the era between the Potsdam and Trenton, and are commonly termed Calciferous. A peculiarity of these limestones is their great richness in limonite or brown hematite ores, which form a large part of the charges of the many blast-furnaces situated on their outcrops. The mines from which the ores are obtained are (properly speaking) only pits or quarries, from which the ore is extracted by means of picks or shovels, powder being rarely employed. The ore does not occur casually at any point in the limestone, but forms regular lines, following apparently the 'outcrops of certain beds. In Lehigh County, Penn., where I have been engaged on the Geological Survey of' the State, during the past season, there are three or four of these lines. During the progress of the survey I was much struck by the fact that the two most important and promising lines of outcrop were, one at the base of the crystalline schists (forming the South or Lehigh Mountain), and overlying the Potsdam sandstone conformably; the other, near the line of junction of the calciferous limestone with the slates of the Cincinnati epoch. The mines along these two lines, following the topography of the country, were in place, richer and more permanent than those of the belts between, which were generally leaner. A peculiarity of these two lines of outcrop, and one to which I particularly desire to draw attention, is the occurrence of what I at first mistook for a highly altered slaty limestone, but which subsequent analysis proved to consist in great part of damourite (hydrated potash mica). The following are analyses of this damourite slate I. From Fogelsville, Lehigh County, within a few hundred feet of the contact of limestone and slate, by Dr. F. A. Genth. II. From Hensingerville, Lehigh County, within 300 feet of gneiss, by Mr. Sydney Castle, of the University of Pennsylvania. III. From Allentown, Lehigh County, within 150 feet of con-

Jan 1, 1875

By R. J. Quigg, G. S. Doble

Commercial stress -relieved TD Nickel bar was shown to retain room- and elevated-temperature tensile strength after exposure up to 2501°F. Cold swaging increased both room -temperature and 2000°F tensile strength. After annealing at 2500°F the strengthening due to swaging was retained at 2000°F hilt eliminated at room temperature. Annealing produced changes in hardness and X-ray half peak width indicating the presence of recovery processes as 1071° as 1000°F but no recrystallization of swaged material was noted at any temperature. In contrast to swaging, rolling induced a recrystal-lized structure after annealing. The tensile strength of this recrystallized structure was comparable to the cold-worked condition. High-temperature tensile properties of as -received bar were highly anisotropic with the transverse tensile strength being one fifth the longitudinal value. The aniso-/ropy is affected by working direction and may he partially reversed by changing the direction of metal flow. The divergence in tensile strength, beginning above 550°F or- approximate one third the absolute melting point, is strain-rate dependent. T D Nickel is a commercial dispersion-hardened alloy containing 2 vol pct thoria. The dispersion, consisting of spherical particles 0.030 to 0.050 in diameter with an interparticle spacing of less than 1 is reported to maintain stable properties up to 2400°F.1 This stability of second phase results in maintenance of elevated-temperature strength at higher temperatures and longer times than normal nickel-base superalloys.2 The purpose of this paper is to describe the effect of various mechanical working operations on the strength and microstructural stability of TD Nickel bar. MATERIAL AND PROCEDURES All material used in this study was commercial TD Nickel bar. This material is produced by a chemical process which results in a nickel powder containing a dispersion of thoria particles. The powder is then pressed, sintered, extruded, and subsequently worked to bar stock. Three starting materials from three separate lots were used: as-extruded bar. 1-in.-diam stress-relieved bar, and 1/2-in.-diam stress-relieved bar. Since TD Nickel bar stock is cold-worked without a recrystalliza-tion anneal, the accumulated deformation or degree of cold work in these materials increases as the bar diameter decreases. Some of the 1/2-in.-diam bar was swaged to 1/4 in. diameter at room temperature in order to produce an as-worked condition for comparison with the stress-relieved stock. Tensile testing was performed on an Instron Tensile Tester at a constant crosshead speed of 0.020 in. per min. The 0.2 pct offset yield strength was measured from the load-crosshead movement plot. Specimen gage dimensions were 0.080 in. in diameter by 0.40 in. in length, producing a strain rate of approximately 0.050 min-1. Specimens were tested in air and heated within a resistance-wound furnace controlled to ±5°F. A 15-min soak at temperature was employed before testing. Samples were heat-treated in air and specimens machined after exposure with sufficient material removed to eliminate any surface contamination. X-ray line breadth was determined from a diffractometer scan of a transverse face of a bar using copper K, radiation. Metallographic preparation utilized standard mechanical polishing with Carapella's etch. Specimens for electron microscopy were electropolished in a 1:7 sulfuric/methaol solution and chromium-shadowed collodion replicas prepared. RESULTS AND DISCUSSION I) Effect of Elevated-Temperature Exposure on the properties of TD Nickel. The effect of various elevated-temperature exposures on the room-temperature tensile strength of TD Nickel is shown in Table I. In the unexposed condition the tensile strength, reduction in area, and hardness all increase with increasing accumulated deformation while the elongation decreases. After exposure at 2500°F the strength of all three materials decreases to about 65,000 psi and the elongations increase slightly. The apparent increase in strength of the 1-in. bar after a 2000°F treatment is probably experimental scatter. These results indicate that the room-temperature strengthening due to additional deformation is annealed out upon elevated-temperature exposure. In contrast to the room-temperature data, the 2000°F tensile strengths increase in order of increasing deformation even after exposure. Although some loss of strength occurs after exposure, much of the effect of working is still maintained at 2000°F. The room-temperature hardness after various

Jan 1, 1965

By Hans Lundberg, Theodor Zuschlag

Based upon an instrumental improvement, a new development has taken place in the art of electrical prospecting, and some remarkable results have already been obtained with regard to potential exploration. In order to visualize the importance of this development, it is deemed advisable to review briefly the fundamental facts about potential surveys. Potential exploration may be carried out qualitatively or quantitatively. Qualitative investigations are made by determining and plotting on a map points of equal potential, whereby any anomalies are revealed, without, however, much clue to their magnitude. Quantitative investigations determine the variations of potential or potential drop, and thus show not only the location of the anomalies, but also their magnitude. Figs. 1 to 6 illustrate the influence of simple types of ground inhomo-geneities, assuming one effective exciter potential only. Such a condition can be closely realized by connecting an electric current source to two electrodes, one of which is located at a great distance. Assuming uniform ground resistivity, the resultant potential distribution mar be represented by concentric spheres. Any change from the normal condition causes a characteristic distortion of the spheres, which becomes different for different types of resistivity variation. The series of Figs. la to 6a illustrates schematically results of qualitative investigations and series lb to 6b results of quantitative investigations. Figs. 1 and 2 picture the well-known case of local resistivity variations normally encountered in ore prospecting. Figs. 3 and 4 show the reactions caused by more or less vertical resistivity contacts and Figs. 5 and 6 refer to the problem of ground-water and bedrock investigations where the resistivity contact is horizontal or nearly SO. It is evident from Figs. 5a and 6a that qualitative measurements do not permit an identification of such general geological features as widespread horizontal strata, because the resultant contraction or expansion of the equipotential circles at the surface cannot be recognized without quantitative determinations. On the other hand, qualitative measurements are well suited for the exploration of local or lateral resistivity

Jan 1, 1932

By John M. Tinsley, Calvin D. Saunders, H. K. van Poollen

In the past few years much con-sideration has been given to the evaluation of the effect of hydraulic fracturing on the productivity of wells. Generally, these studies included the evaluation of fracturing materials, fracture extension and formation damage due to the use of various fracturing fluids. Only little consideration has been given to the characteristics, and in particular the flow capacity, of the fracture itself and its effect on well productivity. This paper presents the results of laboratory investigations pointed toward fie evaluation of the efficiency of various fracrures with special emphasis on the flow capacity of these fractures. Data presented in this paper are the results of both an electrical model study and physical testing. Under consideration are (I) effect of overflush, (2) premature production of well after treatment, (3) "tailing-in" with coarse sand near the end of the treatment, (4) effect of propping agent size and concentration, (5) reduction in effective frac-ture permeability caused by formation caused by formation fines, silt and clays, and (6) effect of various fluids on formation strength and competency. The results of this investigation indicate that the flow capacity of a fracture is affected by any or all of the various parameters mentioned above. The authors believe that a better understanding arid utilization of these factors should result in more efficient formation fracturing. INTRODUCTION Hydraulic fracturing has become almost a standard practice of many companies for stimulating production from old and new wells. Although most companies utilize this service, techniques of application vary widely between companies and areas. Probably too often when a well in an area responds favorably to a particular technique all future wells in the same area are treated in a similar manner. Possibly a modification of the technique would result in a further production increase. Variables, of which many are extremely difficult to evaluate from field results, hamper the selection of procedure changes. Attempts are being made by a number of organizations to analyze statistically treating techniques from production data. This is a very worthy and necessary approach but very possibly laboratory investigations may aid in evaluating some of the variables which tend to affect the results of a fracturing treatment. Some of the factors cannot be studied from practical field experience and only laboratory tests can show the possibilities which might exist. One of the factors which appears to be of major concern today is the flow capacity of the created fracture and how it can be changed. Papers on this general subject have been primarily concerned with the size of propping agent and the extent of fracture. Papers have also been written on the possible permeability damage to formations by fracturing fluids. In addition, it might be possible that another type of flow restriction is prevalent. This would be a restriction of flow through a sand-packed frac- ture caused by foreign materials integrating within the propping agent. This paper presents preliminary data obtained in an attempt to evaluate the effect of some factors affecting flow through sand-packed fractures. No attempt is being made to offer a fracturing technique adaptable to all areas and conditions, but to furnish data tending to show the possible effects which might be caused by variations in procedures and materials. PROPPING AGENT PERMEABLLITIES A hydraulically induced fracture containing sand as a propping agent may theoretically be classified as a packed-sand system. The flow of fluids through such packed systems has been the subject of much research. Although there have been numerous methods proposed for the evaluation of such systems, most writers agree on the general properties affecting their flow capacity or permeability. These properties include porosity, particle size, sphericity and the roughness of the particle. In some methods of evaluation . the particle size and sphericity terms are combined to produce an equation which is a function of the surface area of the particles. In this study the permeability of various fracturing sands was both measured and calculated. The apparatus for the permeability measurements consisted of a 52-in. Lucite tube with a 2.5-in. ID. A screen and drain plug were fitted in the bottom of this tube to retain and hold the sand in place while allowing fluid flow. Two pressure taps consisting of thin, highly perforated

By A. Madrazo

The Standing-Katz method for predicting liquid densities of reservoir fluids has been tested using experimental data of 154 bottom-hole or recombined reservoir fluid samples. New pressure- and temperature-correction curves for the Standing-Katz type correlation are presented which improve the accuracy of prediction. INTRODUCTION The present study was undertaken to investigate the known methods of determining liquid densities and to select one of them which might yield a better correlation if additional data were employed. An appropriate correlation would incorporate the following characteristics: (1) ease of handling in the computations, (2) results within engineering accuracy and (3) data easily accessible. After careful investigation of the different methods, the Standing-Katz correlation1 appeared to have these characteristics. The Standing-Katz correlation for liquid densities of hydrocarbon systems is based upon limited data. The original work, which employs apparent densities for methane and ethane, was based on data of 15 saturated crude oils in equilibrium with natural gas. Therefore, a test of the correlation using additional experimental data would serve either to validate the Standing-Katz correlation or to form a basis for corrections if such were necessary. PROCEDURE AND GRAPHICAL SOLUTION The data of 154 bottom-hole or recombined reservoir fluid samples were employed to calculate the densities at 14.7 psia and 60°F by the method described in Table 1. Volume contributions for methane and ethane were assigned from the pseudo liquid density plot (Fig. I), but volume contributions for N2, CO2 and HzS were not considered. The densities computed at reference conditions of 14.7 psia and 60°F were then elevated to their respective temperatures and pressures by the use of the correction curves proposed by Standing.' The percentage differences between the experimental values and the calculated values were determined; these samples were grouped into temperature, pressure and density ranges to determine a possible trend. It appeared that, at temperatures above 160°F, the calculated density values were consistently larger than the experimental density values; however, no obvious trend was found for the density and pressure ranges. There is a relationship between the pressure-correction and temperature-correction curves. This relationship, embodied in the temperature-correction curve, can be expressed as follows. The experimental densities of 125 samples above their bubble points were known. From these isothermal data, it was possible to determine an experimental-density difference between two pressures; and (from Fig. 2*), a calculated density difference between the same two pressures was determined. The relative effect of temperature must be considered in the calculated-density values. The effect of temperature can be determined by entering Fig. 3* at the two densities in consideration and obtaining the change in density at constant temperature. This change, or delta density, must be added

By Anton Sawatzky, Erich Vogt

By means of mathematical solutions to the appropriate diffusion equations, we describe the kinetics of the thermal diffusion of hydrogen in Zircaloy-2 for the various temperatures and concentrations encountered in a heavy water moderated reactor. When the hydrogen concentration is below terminal solid solubility only the a Phase is present. Redistributions are then described in terms of the characteristic functions of the difhsion equation. For higher concentrations both the a and 6 phases are present. We assume the two phases to be always in equilibrium. For moderately small hydrogen concentrations exact solutions of the two-phase equation approach the the approximate solutions derived by Sawatzky and for all concentrations the exact solutions exhibit the qualitative features of his result: the two-phase concentration increases with time, everywhere; in the absence of a hydrogen current at the hot end of the sample an a-phase region always exists there; the interface of the a + 6 , a-phase boundary moves toward the cold md of the sample and the hydrogen concentration is discontinuous at the interface. Simultaneous solulions of the a and a + 6 hydrogen distributims and of the concomitant interface motion are obtained and compared to the observations of Sawatzky and Markowitz. The kinetics of the hydrogen diffusion process are shown to lead to m apparent heat of transport of the a phase which is lower than the actual value (even for samples with long anneals) thus resolving at least partially the disparity between experimental measurements of this quantity. A number of recent papers1"4 have reported measurements on the diffusion and redistribution of hydrogen in Zircaloy-2 under temperature and concentration gradients. These studies were instigated by problems arising from increasing use of Zircaloy-2 as a fuel element cladding material in pressurized-water power-reactors. The Zircaloy-2 picks up hydrogen during the operation of the reactor: the consequent precipitation of zirconium hydride in the Zircaloy-2 has pronounced effects on its mechanical properties. The Purpose of the present Paper is to describe the kinetics of the thermal diffusion of hydrogen in Zircaloy-2 for the various hydrogen concentrations and temperatures likely to be encountered in reactors. When the hydrogen in the Zircaloy-2 is entirely in the solid solution phase (a phase), the differential equation for thermal diffusion is well known and the redistribution can be described by standard mathematical methods some of which are given in Section 11 below. The treatment of the a + 6 (hydride) region differs from the earlier treatment of sawatzky3 by taking into account several modifications of the two-phase diffusion equations as suggested to us by Markowitz4 and Kidson.5 Even with the modifications the results obtained in our more complete treatment are substantially the same as those found by Sawatzky. As we show, the difference between the results of sawatzky3 and kIarkowitz4 is largely due to the difference in the geometry of their experiments. In the next section we derive the modified two-phase equation for arbitrary geometry. The exact solution of this equation is given in Section III for linear and cylindrical geometry. It is shown that Sawatzky's approximate solution is quite accurate for almost all the temperatures and hydrogen concentrations which are actually encountered. In Sawatzky's approximate theory the hydrogen concentration everywhere in the two-phase region increases continuously. As his paper pointed out, this result, together with hydrogen conservation, implies that in a sample with no hydrogen current flowing into the hot end a two-phase region is always accompanied by a single-phase region at the hot end of the sample. The net hydrogen gain in the two-phase region is supplied by the decrease of hydrogen in the single-phase region and by the movement of the (a, a + 6) boundary toward the cold end of the sample. Hydrogen conservation at the (a, a + 6) boundary leads to a discontinuity in the concentration and its derivative there. In Section IV it is shown how these qualitative features of the thermal diffusion kinetics arise from the simultaneous solution of the a-phase differential equation and a + 6 phase equation. Methods derived by us previously for the solution of the redistribution in both phases and the accompanying motion of the boundary are used to obtain approximate solutions valid for large times. The solutions account well for the observed redistributions of Sawatzky and Markowitz. It is shown how the continuing motion of the (a, a + 6) boundary leads to measured values of the heat of transport lower than the actual value, even for specimens with relatively long anneals.

Jan 1, 1963

By R. I. Jaffee, E. S. Bartlett, D. N. Williams

The oxidation resistance and fabricability of molybdenum powder-metallurgy alloys containing up to 20 wt pct nickel in the form of a fine dispersion were studied. The effects of dispersion distribution and of amount and type (pure nickel or nickel compounds) of additive were considered. A definite improvement in oxidation resistance was observed, but the amount of improvement fell far short of requirements for an oxidation-resistant alloy. Fabricability by hot-rolling was limited. INVESTIGATIONS at Ohio State university1 and Battelle Memorial institute2 have indicated that the attainment of a truly oxidation-resistant molybdenum-base alloy for high-temperature service, with the coincident retention of high-temperature strength and toughness, will be a difficult, if not impossible, feat. Among the most promising alloy systems studied was the molybdenum-nickel system shown in Fig. 1. Alloys in this system show good oxidation resistance at temperatures well above the normal melting point of molybdenum trioxide because of the regenerative formation of protective nickel-molyb-date (NiMoO4) on the surface of the alloy during exposure at high temperatures. Unfortunately, the required alloy content to obtain oxidation resistant molybdenum-nickel alloys far exceeds the limits of the narrow terminal solid-solution boundary, and closely approaches the peri-tectic composition involving the brittle intermetal-lic compound, MoNi. Because of the peritectic reaction, fusion alloys are characteristically brittle, since the MoNi phase, being the last to form, tends to occur as a continuous grain-boundary network around each molybdenum grain. An added problem with this system is that the protective nickel-molybdate layer formed at high temperatures is unstable, undergoing one or more allotropic modifications upon cooling. The volume changes associated with this modification during cooling are such as to cause violent expulsion of the protective molybdate coating from the surface of the piece. This is, of course, quite detrimental in material exposed to cyclic temperature during service. The research reported here resulted from an attempt to overcome the aforementioned problems associated with the molybdenum-nickel alloys primarily by controlling the amount, size, and location of the MoNi phase. By using powder-metallurgy techniques of alloy preparation and sintering the blended molybdenum-nickel powder mixtures at a temperature below the peritectic reaction temperature, molybdenum-nickel alloys with a randomly dispersed MoNi phase were produced. MATERIALS The molybdenum powder used in the preparation of alloys for this study was commercial hydrogen reduced, minus 325-mesh (Tyler) material. Master alloys, by which nickel was added, consisted of elemental carbonyl nickel powder (12 average particle size), an alloy of 50 wt pct Ni-50 wt pct Cr, and compounds of MoNi, Ni,Si, and Ni2B. The nickel-chromium powder was prepared by filing a vacuum-arc-melted ingot, separating impurities magnetically, and screening to minus 200-mesh. The MoNi powder was prepared by pulverizing a hydrogen-sintered powder-metallurgy compact to minus 325-mesh material. Further sizing of this powder for study of effects of dispersion distribution was accomplished by air classification of the minus 325-mesh powder. The Ni2Si and Ni2B powders were prepared by crushing vacuum-sintered powder-metallurgy compacts to minus 200-mesh material. EXPERIMENTAL PROCEDURE Specimen Preparation—The general procedure followed in the preparation of alloys for testing is described as follows: 1) Blending. Either hand-blending of the powders in a ceramic mortar and pestle for X 1/2 or mechanical blending was used. Hand-blending seemed preferable for optimum homogeneity. 2) Compacting. Most of the blended powders were pressed to green compacts at pressures of 15 tons per sq in. in a single-action die, although some were pressed at 80 tons per sq in. A 1 X 11/4 X 1/4-in. green compact was the standard size for oxidation test material, and 7 X 1/2 X 1/4-in. compacts were used for fabricability test specimens. 3) Sintering. All green compacts were sinteredat

Jan 1, 1959