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By M. G. Nicholas

The influence of deformation, relative movement and surface cleanliness on the strength of room -temperature "interparticle" bonds between copper surfaces has been studied. No bonding resulted when clean surfaces were merely pressed together, even under pressures of 50,000 psi. Bonding resulted, however, when clean surfaces were simultaneously pressed and moved relative to each other, some bonding occurring no matter how small the pressure or relative movement. Exposure of the clean surfaces to various chemicals inhibited bonding, none at all being produced by small relative movements. The size of the movements which first produce bonding between exposed surfaces depends on the nature of the chemical, being less than 0.002 in. for cleansing reagents and greater than 0.004 in. for lubricants, water and hydrogen sulfide. It is concluded from the experimental data that the prime requirement for bonding is the dispersal of surface films such as oxides and adsorbed contaminants. THE formation of interparticle bonds during the room-temperature compaction of powder metallurgy components greatly increases the ease of handling in subsequent production operations prior to sintering. The strength of unsintered compacts follows the same general trends as their density and hardness, but quantitative data are extremely Scarce. Quantitative correlation of the data on the overall strength of a compact with that of the individual interparticle bonds is virtually impossible due to the extremely complex geometry of powder compacts. Qualitatively, however, the strengths of unsintered compacts can be correlated with variations in parameters known to influence the extent of cold bonding, and hence interparticle bonding, such as surface cleanliness, relative movement, and deformation of the mating surfaces. Kuzmic and seelig4 found that contamination of powder particle surfaces with lubricants reduced the strength of unsintered iron and copper compacts. Interparticle shear has been shown to promote bonding by Train and Hersey7 while Gregory has shown that die rotation is beneficial. Eilender and schwalbe6 concluded that most bonding occurred during the early stages of pressing iron powder compacts when interparticle shear is one of the principal processes occurring. mile there can be little doubt that these and other factors, such as particle size and shape, affect the extent of interparticle bonding produced by compaction, evaluation of the influence of individual factors is not easy. Particle deformation and relative movement, for example, occur simultaneously during compaction, making any precise measurement of their relative influences difficult. Because of these and other difficulties encountered in studying interparticle bonding in actual powder compacts, the approach adopted in this study was to

Jan 1, 1963

By M. J. Marcinkowski, A. Szirmae, R. M. Fisher

Room -temperature hardness measurements obtained from single and polycrystalline samples of a 47.8 at, pet Cr-Fe alloy which were aged for various times al 500°C show a two-fold increase over that of the unaged alloy after annealing for 1000 hr. A detailed examination of the deformation markings in the neighborhood of the hardness imbressions reveals that twinning becomes an increasingly more important mode of deformation as aging proceeds. this observation is shown to be inconsistent with the Proposals that the transformation is eve of order-disorder On the other hand, the results are in agreement with previous observations of Fisher et al. of a coherent chromium-rich precipitate which forms in an iron-rich matrix as a result of a miscibility gap in this alloy system as proposed by Williams . Using the coherent precipitate hypotlzesis as a model, a detailed analysis of the various possible strengthening contributions to both the slip mid twinning stresses is made. In the case of' slip, lattice friction within the chromium-rich phase and the chemical energy associated with the interface between the two phases contribute about 60pet to the total strength. The contributions from coherency strains and modulus differences are thought to contribute the remaining 40 pet of the strength but are difficult to evaluate because of uncertainties regarding the flexibility of the dislocation line. All of the factors have nearly the same or else a smaller effect on the twinning stress in the aged alloy. Twinning is never observed in the unaged alloy because the twinning stress is much higher- than that for slip. With increased aging times, the various contributions to the total stress for both twinning and slip increase, but most of those for slip increase much more rapidly, so that, in the fully aged alloy, it surpasses the stress for twin propagation. When a twin is nucleated by the chance occurrence of an internal stress concentration during a test, the subsequent twin burst results in a low hardness reading. FeRNTIC Fe-Cr alloys from about 15 to 80 at. pet Cr content show considerable change in properties such as hardness, electrical resistivity, saturation magnetization, and so forth, after aging in the vicinity of 500°C.* The most marked change is a large increase in hardness accompanied by a sharp decrease in ductility, so the phenomenon has often been referred to as the 475°C (885°F) em-brittlement problem. Changes in microstructure are rather subtle and most investigators have not been able to observe any X-ray diffraction or metal-lographic changes during aging. There is little doubt that the phenomenon is inherent to the Fe-Cr binary system and is not directly related to the formation of a phase. Two distinct schools of thought have developed during the past decade concerning this problem. Masumoto, Saito, and sugiharal have concluded, from their own specific-heat measurements, that atomic ordering occurs in this temperature range. Pomey and Bastien2 have also attributed the changes in physical properties with aging in the neighborhood of 500°C to atomic ordering. In addition, Takeda and Nagai3 claimed to have found X-ray verification for superlattices corresponding to the compositions FesCr, FeCr, and FeCr3. However, all known attempts to observe superlattices in Fe-Cr alloys using neutron diffraction, which should be much more sensitive, have been unsuccessful. These have been reported by Shull et al.4 for 25 at. pet Cr, williams5 for 75 at. pet Cr, and Tisinai and samans6 for a 28.5 at. pet Cr. steel. The second and more prevalent opinion ascribes the 475°C embrittlement phenomenon to the formation of a coherent precipitate due to the occurrence of a miscibility gap in the Fe-Cr system below about 550°C. This latter concept was first indicated by the results of Fisher, Dulis, and Carroll,7 who were able to extract fine particles about 200Å in diameter from samples of 28.5 at. pet Cr steels aged from 1 to 3 years at 475°C. The extracted material was found to be nonmagnetic, to have a bee structure with a lattice parameter between that of iron and chromium, and to contain about 80 at. pet Cr. Williams and paxton8 and williams5 confirmed these results and first explicitly proposed the existence of a miscibility gap below the a region in the equilibrium diagram. Alloys aged within this gap

Jan 1, 1964

By E. S. Machlin, S. Weing

GRAIN boundary stress relaxation has been the subject of several investigations in recent years, but as yet the phenomenon is not well understood. One of the major difficulties has been the lack of a sufficient amount of data with which to evaluate any proposed mechanism. Little information is available on the effect of small amounts of substitutional solutes on grain boundary stress relaxation. It is with this important phase of the problem that this investigation is concerned. The influence of substitutional solutes on grain boundary stress relaxation has been recently investigated in copper by Pearson: and in aluminum by Dorn et al.' Pearson studied the effect of zinc, gallium, germanium, and arsenic on the relaxation peak of OFHC copper.* The pure OFHC copper decreased the peak intensity and a second peak appeared at a higher temperature. This latter peak was termed the alloy grain boundary peak. At the lowest binary concentration studied, approximately 1 atomic pct, the primary peak was almost completely obliterated. Pearson found that the activation energy calculated from the alloy grain boundary peak for all solutes, irrespective of the concentration, was 44,000 cal per mol. Pearson concluded that the increase in activation energy from 33 to 44 kcal per mol is not continuous but abruptly changes from the lower to the higher value. As no attempt was made to investigate the intermediate range of concentration and hence calculate the possible variation of the activation energy for the initial grain boundary peak, this conclusion is hardly valid. In contrast to these results, Dorn et al. studied the effect of zinc, silver, copper, germanium, and magnesium on the grain boundary stress relaxation of aluminum. No change in the energy of activation was observed for binary alloys of the flrst four solutes, but a linear increase was found for increasing concentration of magnesium. Saturation was not found up to the maximum of 1.6 atomic pct. The energies of activation were obtained by plotting the horizontal displacement of the dynamic modulus curve vs temperature for two vibrational frequencies. As the modulus is proportional to the square of the frequency, this requires the measurement of the torsional frequency over a range of temperature. However, the technique does not lead to an unambiguous interpretation of the grain boundary

Jan 1, 1958

By R. W. Ludt, C. C. DeWitt

The use of froth flotation for the separation of minerals has become one of the most important of ore dressing processes. Its particular adaptability to the enrichment of low grade ores has made the process an important factor in the national economy. The methods have been extended to the recovery of a great number of minerals. Among the few minerals which have resisted efforts toward industrial flotation is chrysocolla, a hydrated partly colloidal copper silicate. Chrysocolla, being a product of natural oxidation, has been found to occur in small quantities with many ores which are recovered by flotation methods. In present practice, these small quantities of copper silicate pass off with the tailings and are lost. The advantages to be gained by a satisfactory process for the recovery of chrysocolla is apparent. Any application of principles which points a way toward the satisfactory industrial flotation process for copper silicate would be of advantage. This paper presents an attack on this problem. Two methods for the recovery of chrysocolla have been developed by the United States Bureau of Mines.1,2 They have been successful on a laboratory scale but have been seriously restricted in industrial application by critical requirements in the procedure. In one of the Bureau of Mines methods,' the ore is activated with sodium or hydrogen sulphide in an aqueous solution at a pH of 4. Amy1 xanthate is then used as a collector with pine oil as a frother in the flotation process. An excess of sulphide acts as a depressant and the state of optimum conditions is difficult to control industrially. In the second Bureau of Mines method,2 soap is used as the collector at a pH of between 8 and 9. The diffi- culties with this process are that soap is not a specific collector, that heavy metal or alkaline earth ions cause the formation of insoluble soaps, and that a more acid solution causes the formation of a free acid which does not act as a collector for chrysocolla. The problem of recovering chrysocolla by flotation involves the selection of a suitable collector. The collector molecule must be composed of an active polar group that has an attraction for chrysocolla, and of a hydrocarbon chain. Certain dyes have been shown to have an attraction for certain minerals. Suida3 found that hydrated silicates are colored by basic dyes. Dittler4 showed that chrysocolla, among other colloidal minerals of acid reaction, preferentially takes up such basic dyes as fuchsin B, methylene blue, and methyl green. Endell5 gave information to show that the colloidal material in clay may be determined by its selective adsorption of fuchsin. A simple experiment, likewise, illustrates the difference in the adsorptive power of chrysocolla and of silica for the basic triphenyl methane dyes. When a mixture of chrysocolla and silica is immersed in a very dilute dye solution, less than 5 ppm, the chryso-colla is rapidly dyed and the silica is dyed more slowly. The difference is substantial but one of degree. Dean2 showed that the dyes, crystal violet and toluidine blue, are taken up by quartz in an adsorption type process. The difference in the adsorptive power, however, offers the means by which a new collector may act. To form such a collector, a hydrocarbon chain must be attached to the dye molecule. This involves a process of organic synthesis. Butyl, hexyl, and octyl hydrocarbon chains were selected for substitution in the malachite green molecule. For the purpose of identification, the alkyl-substituted dyes formed are called: butyl-malachite green; hexyl- malachite green; and octyl-malachite green. An outline of the procedure for their synthesis is given in the appendix. It is generally recognized in the preparation of this type of dye that the chemical structure of some of the dye molecules varies. However, a uniform formula is attributed to the dye. Such a procedure has been followed in specifying the structure of these alkyl-substi-tuted malachite green dyes. The structure is given on the basis of their properties as an homologous series of dyes, on their method of preparation, and on the purity of intermediates used. Structure of substituted alkyl malachite green is: C6H4 N(CH3)2 p-R C6H4 CH C6H4 N(CH)2 Procedure The flotation cell is a Bureau of Mines 100-g, batch unit provided with an air inlet at the bottom above which is a variable speed agitator. The agi-

Jan 1, 1950

By Frank Tolonen

IRON-ORE beneficiation is becoming of vital importance to the Lake Superior region, since only a few decades will be needed to exhaust the direct shipping ores even if generous allowances are made for discoveries of new orebodies. If the region is to continue as the chief source of ore to the steel industry of the United States, it must concentrate or otherwise beneficiate the enormous tonnages of available iron formations. A beginning along this line has already been made. About one-fifth of the total shipment, even now, is the product of some sort of concentrating process, while another fifth is improved in physical structure by crushing, screening, drying, sintering, or some other similar method. The amount of material amenable to these processes is limited, however; and, in order to be able to utilize the billions of tons of iron formations that cannot be so beneficiated, an intensive study of their nature and concentration possi-bilities is necessary. As long as high-grade ores are available in ample quantities, ore dressing is economically impossible, but as soon as the supply nears exhaustion it becomes necessary. At first the products of ore dressing must meet as nearly as possible the same specifications as the rich ores in order to be adapted to the reduction processes already established. The future requirements as to quality will depend on the one hand upon the ability of the ore dresser to eliminate undesired constituents and charac-teristics in the material, and on the other upon the adaptation of the reduction processes to the product that can be economically supplied. A better understanding of the blast furnace and other reduction reactions, and improvements in the preparation of raw materials, should enable the Michigan districts to continue to supply ore for a long time to come. The study and testing of the iron formations necessary to bring a utilization of the low-grade ores, though requiring time and effort on the part of all concerned, should not be postponed, especially since the economic situation forces the use of the highest grade ore in preference to the leaner material.

Jan 1, 1933

By Wilbur I. Duvall, Wilson Blake

The microseismic method of detecting instability in underground mines was developed by the U.S. Bureau of Mines (USBM) in the early 1940's. ,3 The method relies on the fact that as rock is stressed, strain energy is stored in the rock. Accompanying the buildup of strain energy are small-scale displacement adjustments that release small amounts of seismic and acoustic energy. These small-scale disturbances, which can be detected with the aid of special geophysical equipment, are called micro-seisims or self-gene rated rock noises. It was further determined that as failure of rock is approached, the rate at which rock noises are generated increases. Thus, by monitoring a rock structure at intervals and plotting rock noise rates vs. time, a semi quantitative estimate of the behavior and stability of the structure can be made. Since sufficient use of the microseismic method is still being made by various mining and construction companies, USBM undertook a comprehensive review of the method and a study of the fundamental properties of rock noises. As all prior work on rock noises has been done with resonant-type geophones, which prevented any analysis of their vibration records, it was necessary to develop the instrumentation and field techniques in order that their properties could be investigated, such as their frequency spectrum and absorption characteristics, and to determine if both P and S-waves are generated by a rock noise. The aim of this program is the design of microseismic instrumentation which can be better utilized as an engineering tool than the presently available microseismic equipment. This new design, based on the basic properties of rock noises, should allow better utilization of these phenomena in the study and location of zones of incipient instability in both underground and open-pit mines. EXPERIMENTAL PROCEDURE To study the waveform of rock noises, it was necessary to develop a microseismic system with a broad bandwidth. To achieve high sensitivity and broad frequency response, commercial ceramic accelerometers were used. The present broad-band microseismic system consists of accelerometers as geophones, low-noise preamplifiers, high-gain amplifiers, and an FM magnetic tape recorder. This seven-channel system has a flat frequency response from 20 to 10,000 Hz, a noise level of less than 2.0 kv, and a dynamic range (including manual set attenuation) of greater than 100 db; it can detect signals with acceleration levels as low as 2 ug. The entire system is solid state and hence battery operated and portable (Fig. 1) Analysis procedures consist of playing back the 30-in-per-sec (ips) magnetic tape recordings at 1 7/8 ips to expand the time scale of a recorded rock noise event and then recording this on a high-speed direct-writing oscillograph. The oscilIographic records are then digitized and run through Fourier integral analysis computer programs to determine the frequency spectrum of a rock noise event. The oscillographic records are also examined visually to determine if both P and S-waves can be recognized in a rock noise waveform. Broad-band microseismic recordings have been made at field sites in a wide variety of rock types and in both underground and open-pit mines. Sites include the Kimbley Pit, Ruth, Nev.; the Galena Mine, Wallace, Idaho; the Colony Development Mine. Grand Valley, Colo.; the Cliff Shaft Mine, Ishpeming, Mich; and the White Pine Mine, White Pine, Mich. DATA AND DISCUSSION Analyses of the recorded data have shown that rock noise frequencies are very broad. Fig. 2 and 3 show typical rock noise events and their frequency spectrums. In addition, it is evident from these figures that the wave form of a rock noise is very complex. The wide frequency variation, 50 to 7500 Hz, is due to many variables; the effect of travel distance is the only one examined in this study. The higher frequency components of the wave are rapidly absorbed with distance or increasing travel time. Fig. 4 shows the change in waveform resulting from an additional travel distance of 195 ft. From these data, it is apparent that a resonant-type microseismic geophone cannot respond to all frequencies generated by a rock noise, and in spite of the fact that the tuned geophone is more sensitive at resonance, a geophone with less sensitivity but broader band width is much more effective in detecting rock noises. In addition, a study of broad-band microseismic records shows that both P and S-wave arrivals are easily detected, as shown in Fig. 5. All records analyzed to date show that most of the energy is in the S portion of the wave; hence, microseismic geophones should be well

Jan 1, 1970

By J. R. Finlay

The Cæur d'Alene silver-lead mining district of northern Idaho is probably best known to the general public as a seat of labor-troubles. So far as the writer is aware, little has been written and little is known about its geology and resources. People interested in lead-smelting are, of course, cognizant of the economic importance of the region, but they have not communicated much of their knowledge to the public. Exact figures as to the total output of the district are not obtainable, but the following estimates, covering the entire output of the 15 years during which the mines have been operated, are believed to be approximately correct: Group of Mines. Product. Wardner Group, including the Bunker Hill and Sul livan, Empire State-Idaho, Last Chance, Sierra Nevada, bur d'Alene Development Co... . $17,500,000 Cafion Creek Group, including the Gem, Frisco Con solidated, Granite, Standard, Mammoth, Hecla, Tiger-Poorman, Custer and Bell,.... 35,000,000 Mullan Group, including the Morning, You Like and Gold Hunter,........7,500,000 $60,000,000 This output covers the period of discovery and early struggles, and several periods of stagnation caused by strikes and other serious labor-troubles. In 1900 the output of the district was fully $10,000,000, and this figure would have been considerably increased in 1901 had not a curtailment of production been forced by the condition of the lead-market. In 1901 the product was about 150,000 tons of concentrates, with a gross. value of $8,250,000.

Jan 1, 1903

By A. Boltax

Precipitation processes occurring during both furnace cooling and aging of copper-iron albys were studied by means of electrical and magnetic measurements. On furnace cooling, two distinct stages in the precipitation process were detected; one occurring above and the other below 850° C. The kinetics of precipitation from quenched alloys were studied between 200° and 700°C. The reaction appears to be consistent with the concept of tmcleation of precipitate particles at dislocation loops formed by the clustering of quenched-in vacancies. A study Of in copper-iron alloys is particularly interesting because the combination of magnetic and electrical properties in these allovs provides a quantitative means of following the course of the precipitation reaction. (The details of precip-

Jan 1, 1961

By R. A. Grange, H. M. Stewart

Man.; steel parts may crack if quenched directly into a bath near room temperature, but not if quenched at a temperature just above the range where martensite forms and then allowed to cool slowly to room temperature. This latter procedure, which is the basis for such modern hardening techniques as "martempering" and "isothermal quenching," may entail some sacrifice in depth of hardening but very little, if any, in intensity of hardening. In planning such treatments, it is necessary to know the upper limit of the martensite range, and often desirable to know the proportion of martensite that would form on cooling to any lower temperature; furthermore, the tendency of a particular steel to crack when quenched is unquestionably associated with the temperature range of martensite formation, and consequently knowledge of this range aids in selecting the optimum composition for a given application. Certain puzzling phenomena associated with the properties of quenched and tempered steel may be at least partly clarified as the manner in which martensite forms is more fully understood. Information on the temperature range of martensite formation, particularly with respect to how much martensite results from quenching to a given temperature, is lacking for most commercial types of carbon and low-alloy steel. These considerations led us to study martensite formation in 14 carbon and low-alloy steels. The resultant data may be directly used in the following ways: (I) for selecting the lowest quenching temperature at which no martensite will form; (2) for selecting the highest quenching temperature at which virtually all marten . site will form, thereby avoiding quenching to an unnecessarily lower temperature with attendant danger of cracking; and (3) in producing a mixture of tempered martensite and bainite, which in high-carbon steels has been found to possess somewhat better ductility than tempered martensite, yet does not require the full transformation time necessary for a completely bainitic (austempered) structure. PART I. OBSERVATIONS OF MARTENSITE FORMATION IN FOURTEEN CARBON AND LOW-ALLOY STEELS Transformation of austenite to pearlite or bainite can be conveniently studied by observing the change that occurs over a period of time at constant temperature; such studies are the basis of the isothermal transformation diagram (S-curve). This isothermal technique is not applicable to martensite formation, which occurs within a time interval too small to measure, at least by any ordinary means. For all practical purposes, therefore, martensite may be regarded as forming only during cooling and not during a period of time at constant temperature. As austenite is cooled below

Jan 1, 1947

By H. M. Stewart, R. A. Grange

Man.; steel parts may crack if quenched directly into a bath near room temperature, but not if quenched at a temperature just above the range where martensite forms and then allowed to cool slowly to room temperature. This latter procedure, which is the basis for such modern hardening techniques as "martempering" and "isothermal quenching," may entail some sacrifice in depth of hardening but very little, if any, in intensity of hardening. In planning such treatments, it is necessary to know the upper limit of the martensite range, and often desirable to know the proportion of martensite that would form on cooling to any lower temperature; furthermore, the tendency of a particular steel to crack when quenched is unquestionably associated with the temperature range of martensite formation, and consequently knowledge of this range aids in selecting the optimum composition for a given application. Certain puzzling phenomena associated with the properties of quenched and tempered steel may be at least partly clarified as the manner in which martensite forms is more fully understood. Information on the temperature range of martensite formation, particularly with respect to how much martensite results from quenching to a given temperature, is lacking for most commercial types of carbon and low-alloy steel. These considerations led us to study martensite formation in 14 carbon and low-alloy steels. The resultant data may be directly used in the following ways: (I) for selecting the lowest quenching temperature at which no martensite will form; (2) for selecting the highest quenching temperature at which virtually all marten . site will form, thereby avoiding quenching to an unnecessarily lower temperature with attendant danger of cracking; and (3) in producing a mixture of tempered martensite and bainite, which in high-carbon steels has been found to possess somewhat better ductility than tempered martensite, yet does not require the full transformation time necessary for a completely bainitic (austempered) structure. PART I. OBSERVATIONS OF MARTENSITE FORMATION IN FOURTEEN CARBON AND LOW-ALLOY STEELS Transformation of austenite to pearlite or bainite can be conveniently studied by observing the change that occurs over a period of time at constant temperature; such studies are the basis of the isothermal transformation diagram (S-curve). This isothermal technique is not applicable to martensite formation, which occurs within a time interval too small to measure, at least by any ordinary means. For all practical purposes, therefore, martensite may be regarded as forming only during cooling and not during a period of time at constant temperature. As austenite is cooled below

Jan 1, 1947

By Paul A. Beck, M. N. Parthasarathi

By determining the (220) pole figure for OFHC copper rolled to 96 pct R. .A., the occurrence of four texture components of the type (135) [211] was confirmed. It was found that the total volume fraction of material close to the four symmetrical orientations of this type is larger than the volume fraction of the other components put together. THE rolling texture of copper was described by early investigators1'" as a mixture of components of the (110)[l12] and (112) [11l] types. Other studies, still using the qualitative photographic method of texture determination arrived, instead, at orientations of the type (135) [533] or (135) [211] for copper3'4 and at the closely related "Z-texture" for a fee nickel-iron alloy.5 The prevalence of this type of orientation, near (123) [412], in the rolling texture of aluminum and of copper was later confirmed by means of quantitative diffractometer methods.' However, in a recent paper7 Jones and Fell stated that the (110) [112] and (112) [111] double texture was in better agreement with the measurements of Young's modulus for cold-rolled copper.' These authors also expressed their belief that the "roll texture" can be determined by means of two photographic quasi-fiber texture patterns taken with sheet specimens rotated around the rolling direction and the transverse direction, respectively. Jones and Fell found7 that the results obtained from such patterns for cold-rolled nickel did not agree with any of the orientations mentioned above, but they suggested that the observed diffraction spots may have been brought about by the overlapping of reflections due to the (110) [112] and (112) [11l] double texture components. Jones and Fell concluded that the (123) 14121 type orientation is inconsistent with their patterns. They also stated, without offering any supporting evidence, that this orientation is inconsistent with the (220) pole figure. "Ideal orientations" are often used for a very rough description of the principal orientations encountered in a texture, It is, however, well to remember the fact that, no matter how "accurate", these ideal orientations are only schematic representatives of a continuous distribution9, which often (as in the case of rolled copper) includes extensive orientation spreads. The attempt by Jones and Fell7 to use elastic modulus data in deciding between various ideal orientations in the rolling texture of copper neglects this fact. The inadequacy of two-dimensional "axis density figures" in describing orientation distributions in sheet textures was previously discussed.9 It was also pointed out9 that there is no reliable evidence to prove that orientation distributions derived by the "quasi-fiber method" from rotated sheet specimens are fully equivalent to the corresponding information obtainable from quantitative pole figures. The view that a sheet texture could be adequately determined by means of two photographic quasi-fiber texture patterns is obviously erroneous9. The question as to the consistency with the (220) pole figure of ideal orientations derived from the (111) and (200) pole figures is, on the other hand, certainly very relevant. Since no quantitative (220) pole figure for cold-rolled copper appears to be available in the literature, the following work was undertaken. EXPERIMENTAL METHOD An extruded rod of OFHC copper, 1 in. in diam, was given alternate rolling (30 to 35 pct R.A.) and

Jan 1, 1962

By F. J. Plecity, J. T. Michalak, W. C. Leslie

Isothermal recrystallization and grain growth in zone- and vacuum-melted irons and Fe-Mn alloys, up to 0.60 pct Mn, were studied in the range 480° to 650° C, after 60 pct cold reduction. In initial stages, rate of grain growth and rate of recrystallization of iron decrease with time. The recrystallization is typical of a growth-controlled process, and rate of growth is determined by the extent of recovery. Mn decreases rates of growth and of recrystallizatzon. The recrystallization process changes at about 0.30 pct Mn and nucleation may become time-depetzdet~t. In recent years, considerable effort has been expended in determining the effects of solute elements on recrystallization and boundary migration in fcc metals. The results have indicated that the effects produced by single solute additions are dependent upon both the element added and its concentration.'-' In contrast, there have been very few attempts to determine the characteristics of recrystallization and boundary migration in high-purity bcc metals, especially after heavy deformation, and the effects thereon of single solute elements.9-11 This study was undertaken to determine the recrystallization characteristics of various "high-purity" irons and the effects of manganese additions at two levels of base purity. It was hoped that the information obtained would improve our understanding of the recrystallization of pure metals and aid in formulating a theory for the effect of solute elements. The interest was not entirely academic, for the annealing of low-carbon steels, which is of very great commercial importance, is but poorly understood. MATERIALS The compositions of the irons and iron-manganese alloys used are listed in Table I. The zone-melted iron and Fe-Mn alloys were made by Battelle Memorial Institute. Iron S-1 was arc-melted in a water-cooled steel mold in an argon atmosphere. The ingot was forged into a bar, then given two horizontal zone-refining passes in an alumina boat. Iron V-4 was treated in a similar manner, but was not zone-refined. The iron for the zone-melted Fe-Mn alloys was induction melted in vacuum in MgO crucibles and cast into alumina molds. The ingots were forged into bars, machined to shape, and a groove milled down one side of each. The best available electrolytic Mn was placed in the grooves, and the bars were zone melted. The vacuum-melted Fe-Mn alloys were induction melted in this Laboratory in MgO crucibles and poured into cast-iron molds. Iron V-5 was purchased from National Research Corp. in the form of a small vacuum-cast ingot. The low-carbon steel was made by induction melting in air at the U.S. Steel Corp. Applied Research Laboratory. The history of the materials prior to the final cold reduction differed; these details are given in the Appendix. The penultimate grain size of the principal materials was kept in the range ASTM 2 to 4, except for the low-carbon steel. PROCEDURES The cold work prior to the final recrystallization anneal was kept constant at 60 pct. It is known that rolling procedure can influence the kinetics of recrystallization of ironI2; therefore, all specimens were rolled in one direction only, between clean,

Jan 1, 1962

By R. M. Brick

Segregation can occur only in cast alloys that solidify over a range of temperatures with a difference in composition of liquid and solid phases within this range (ignoring monotectic systems and chemical reactions as in rimming steels). Thus a pure binary eutectic alloy should show no segregation unless undercooling occurs for one of the solid constituents of the eutectic; e.g., chill-cast Al-I2 per cent Si alloys. The phasial condition implicitly described above—solidification over a range of temperatures with a compositional difference between solid and liquid—is found in nearly all solid solutions or combinations of solid solutions and eutec-tics, Metastable conditions of solidification of these types of alloys cause coring; i.e., a difference in composition between the center of a dendrite and its periphery. This composition gradient can be detected usually only by microscopic examination of etched structures; it is a "micro" effect. The gradient of more immediate industrial concern is that between the center of a cast section and the surface layers. This gross (macro) effect is usually deter-minable only by sampling of the casting at different points, with chemical analyses of each sample. If the compositional difference is of the same type as in coring, the first parts to freeze being enriched in higher-melting-point constituents, and vice versa, the effect is called normal segregation. When what is apparently the first part of the casting to solidify shows a higher concentration of low-melting-point constituents, the effect is called inverse segregation. These macro effects are quite separate from the micro effect, coring, yet the latter must be described first because it is an essential part of the picture. Coring Solid Solution, Ni-Cu The nickel-copper phase diagram is reproduced in Fig. Ia, in which the solid lines represent the equilibrium liquidus I, 3, 7 and solidus 2, 5, 8, and where the vertical I, 4: 8 represents a 55 per cent Cu alloy. Upon moderately rapid solidification, the first dendritic axes of composition 2 (see Fig. Ib) start to form at a temperature somewhat under I. Solidification continues by growth of the dendritic nuclei, but at temperature 4 the increment solidifying is of composition 5. The rapidity of this crystal growth prevents diffusion of nickel and copper atoms from adjusting the composition of the entire dendrite at 5, which it would be under equilibrium conditions. The average composition of a specific dendrite, or the entire solid phase, at temperature 4 might be that indicated

Jan 1, 1945

By W. Kennedy

THROUGHOUT northeastern Texas we have an extensive series of iron-ore deposits, occupying portions of nineteen counties and having approximately an actual ore-covered area of 1000 square miles. The existence of these ores has long been known. Kennedy* says: "Iron-ore is distributed in profusion throughout Texas, being found almost everywhere except in the level region of the coast." Before this, C. Newell† had mentioned the existence of these ores thus: " Iron is found in abundance in the eastern, northern and middle portions of Texas;" and in 1849 Edward Smith‡ said: " We met with immense hills of iron which were said to be, and appeared to be, of excellent quality, in Cass and Titus counties.. . .. It is well known that Texas abounds with iron of first-rate quality." In 1859, Dr. Shumard? reports that detailed surveys had been made in several counties, and says: " Our labors have demonstrated the important fact that we have a vast iron-region in the eastern part of the state, embracing considerable areas in Cass, Harrison, Rusk, Panola, Smith, San Augustine and Shelby counties. The ore-deposits belong to the Tertiary era and consist chiefly of hematites and limonites, of which there are several varieties. We have also found in this district extensive beds of carbonate of iron." Dr. Shumard gives no very exaggerated description of Cass county§ as it then existed when he says : " Cass county alone is capable of supplying a number of furnaces with an abundance of excellent iron-ore for many years." Of Rusk county he says: "Our de-

Jan 1, 1895

By J. D. Forrester, Erich Sarapuu, T. C. Cheasley

RANKING high in the nation's wealth of natural resources, readily available liquid and gaseous hydrocarbons are nevertheless falling steadily in supply, while industrial requirements for hydro- carbon compounds are greater today than during the peak period of World War II. Theoretically, several processes will increase the future supply of liquid and gaseous fuels, but the practical application of these methods depends on two controlling factors: 1-that enough carbon- bearing material be available to warrant industrial exploitation, and 2-that the given process be physically, chemically, and economically applicable. With regard to the first factor, the Western Hemisphere is fortunately well supplied, see Table I.

Jan 9, 1954

By C. D. Wiseman

THE concept of alloying to increase the strength of metals originated during the bronze age. However, at the present time there is no single theory capable of explaining all of the observed strengthening effects of alloying elements on the mechanical properties. In general, it may be said that solid solutions are stronger than the pure metal and that the strengthening effect increases with increasing alloy content. Various theories for solution hardening have been proposed, the first of which was presented by Rosenhain who suggested that the alloying elements roughened the slip planes, thereby requiring a higher stress to initiate slip. Recent work by French and Hibbard2 confirmed Norbury's3 conclusion that those alloying elements which cause a greater change in lattice parameter have larger effects on hardness. However, a given change in lattice parameter produced by different alloying elements does not cause the same change in hardness. A further refinement was suggested by Dorn, Pietrokowski, and Tietz4 who considered differences in valence between the solute and solvent with the change in lattice parameter to explain the plastic properties of aluminum alloys. Allen, Schofield, and Tate5 further investigated the valency contribution to solution strengthening by testing some copper-base solid-solution alloys having constant electron densities. Tensile tests performed on these alloys gave identical stress-strain curves even though the atomic size effect, which varied by a factor of two, was neglected. The advent of dislocation theory6-8 provided a new and powerful tool capable of explaining many phenomena of plastic deformation and indicated new approaches to solution hardening. The basic con- cept of recent theories is that solution hardening is not due to stresses associated with randomly dispersed solute atoms, but rather to a nonuniform distribution of the solute. This conclusion was reached by consideration of the effective tension present on each dislocation line and the ability of a dislocation to pass an obstacle. cottrell suggested the possibility that the internal stresses due to randomly distributed solute atoms would offer essentially no resistance to the passage of dislocations. He reasoned that an edge dislocation may be considered as a rigid line discontinuity. As the dislocation moved through a crystal, the random stress fields would be equally distributed along its length. Since half of the stress fields would be acting to move the dislocation forward and the other half trying to move it back, the net effect on the dislocation would be zero. Thus the randomly distributed solute atoms would not contribute appreciably to solution strengthening. Mott and Nabarro10 considered the dislocation as a flexible, rather than a rigid, discontinuity. They obtained a simple model for a dislocation moving in a lattice having precipated particles, where the dislocation would actually bend around the obstacle until it would loop back onto itself to rejoin and then continue onward. Their work indicated that the minimum radius of curvature of the dislocation line, under the action of an external stress and in the region of an internal stress, would be such that the dislocation would be unable to pass through a matrix containing small closely spaced precipates by the looping process. The dislocations would tend to remain rather straight, approaching the condition of Cottrell's rigid dislocation. Hence, the strengthening must not be due to random solute atoms; however, it might be due to the concentration of atoms, either as clusters of like atoms or as short-range ordered regions, or to the concentration of solute atoms around dislocations. To date, four mechanisms of solution strength-

Jan 1, 1959

By Persifor Frazer

At a time when all those interested in the iron trade are carefully scanning the horizon for new sources of the raw material, a few words concerning a field, which though not new, has not been hitherto fruitful of statistical information, may be deemed appropriate at this meeting. The district alluded to is the belt of the Middle James River, or in other words, that portion of the ferriferous belts of Virginia lying between Josua Falls and the little settlement of Norwood, in the counties of Amherst and Nelson, and on the left bank of the James River. This region shows unmistakable signs of developing a very considerable market for iron ores and for iron in the future, as well as a tempting appearance of possible productiveness in the former. It, is extremely hazardous to deal in generalizations as to the productiveness or non-productiveness of these measures without a more thorough development than has yet been attained. It is true that they probably constitute an horizon whence comes a part of the marvellous mineral wealth of the northern peninsula of Michigan. But

Jan 1, 1883

By S. L. Lopata, E. B. Kula

A variation of yield and tensile strength with direction has been noted in heat-treated 4340 steel which had been warn-worked by rolling in the austenitic condition prior to quenching. Measurements by X-rays showed a preferred orientation of martensite crystals. Various ideal preferred orientations of martensite were calculated by assuming a preferred orientation for austenite and transforming this to martensite by the Kurdjumov -Sachs and Nishiyama relationships. Comparison with the measured preferred orientation showed that the ideal rolling texture for austenite in 4340 steel could be expressed as a (112) [111] texture with a component of (110) [112]. No evidence was found for any fiber axis in the rolling direction, or fop- a (123) [412] texture. The observed martensite pole figures can be adequately accounted for by these ideal austenite textures and by the Kurdjumou-Sachs or Nishiyama transformation relationships between austenite and martensite. ALTHOUGH preferred orientations are found in cold-rolled steel sheet and in many nonferrous metals, they are not generally encountered in wrought, heat-treated high-strength steels, since such steels are generally not cold worked sufficiently to develop a strong texture, and any texture that is present is removed during heat treatment by the phase transformations taking place. This report gives details on a preferred orientation found in warm-rolled and hardened 4340 steel. In a recent study, a special combination heat-treating and working technique was used in which 4340 steel was deformed in the austenitic condition, and before re crystallization of the austenite could occur, quenched to form martensite.' Since the austenite was unrecrystallized, it was cold worked and hence could have contained a preferred orientation which could be transmitted to the martensite on quenching, and this in turn could be manifested as a directionality of mechanical properties. Such a directionality of properties was found as a result of working, and this prompted an X-ray study of the preferred orientation. Literature Survey— Rolling Texture in Face-Cen-tered-Cubic Austenite—M a preferred orientation is found in a rolled and hardened steel, it is first appropriate to consider what texture existed in the austenite as a result of the rolling but prior to the transformation to martensite. The changes taking place as a result of the austenite-martensite transformation are then considered. In view of the instability of austenite in 4340 steel at low temperatures, no direct determination of the austenite texture was made. However, an estimate of the texture for austenite in 4340 steel may be made by considering the textures found for other face-centered-cubic metals. Barrett' has reviewed the rolling textures for many materials. The most common orientation in face-centered-cubic metals has the (110) planes parallel to the rolling plane and the [112] directions parallel to the rolling direction, or (110) [112]. Other orientations found are (112) [111], as well as (100) [001], (110) [001], and others. Beck and his co-workers, using quantitative pole figures, report that (123) [121],3 later corrected to (123) [412],4 better describes the ideal orientation. smallman5 reported that the ideal preferred orientation for high-purity face-centered-cubic metals is (123) [121], but that there is a transition to (110) [112] as solid solution elements are added. The latter texture tends to occur more readily at lower temperatures. This transition between the two textures was explained by differences in the slip characteristics with concentration or temperature. More recently, Jones and Fell6 concluded that the (123) [412] texture for face-centered-cubic metals could equally well be represented by a mixture of (110) [112] and (112) [111] textures, and hence it had no physical reality. From the above results it can be seen that there is no agreement on the "ideal" texture for fcc metals and, hence, no firm basis for assuming a texture for austenite in 4340 steel. Therefore, the orientations (110) [112], (123) [412], and (112) [111] have been considered in the following.* *The (123) [4121 is identical to the (123) [121] rotated 90 deg. Orientation Relationship between Austenite and Martensite—When martensite forms from austenite, certain crystallographic planes of the martensite are parallel to planes in the austenite. This orientation relationship was first determined by Kurdjumov and

Jan 1, 1960

A knowledge of the principles of punctuation is essential to effective and intelligible writing, for the ease and pleasure of the reader, and even his understanding, may depend upon the choice and the placing of punctuation marks. To 'punctuate' is to mark with stops or points; the word comes from the medieval Latin punctuare (punctuatus), which in turn is derived from the Latin punctum, a point. The purpose of punctuation is to show the manner in which the writing is to be understood; to indicate the relations between parts of a sentence and between successive sentences. To some extent "it does for the eye what vocal stress does for the ear", but especially it marks logical relations. Some punctuation marks, such as those indicating admiration, exclamation, and interrogation, are rhetorical as well as grammatical, but most of the common ones are logical or grammatical. My discussion will be confined to grammatical punctuation in ordinary writing. "The problem of punctuation in text matter", as George Summey * says, "is to employ words, points, and paragraph breaks in such a way as to achieve at the same time clearness, proper distribution of emphasis, and the desired kind of movement." The criticism of the punctuation of a sentence or of a group of sentences is not final until the context, within the paragraph, is read. A paragraph is a sentence or a group of' sentences forming an independent unit of the composition; it represents a unit of thought. A multiplicity of paragraphs produces a choppy effect; on the other hand, paragraphs of excessive length are tiresome, because the belaboring of one unit of thought wearies the reader. The aim should be to

Jan 1, 1931

By Chung Yu Wang, Guy C. Riddle

There are found in nature upward of II2 minerals containing antimony, but only a few of them, listed in Table I, can be considered as antimony ore-forming minerals. Stibnite (Sb2S3), antimony sulphide or glance, is the principal ore of antimony. The oxide ores—cervantite, kermesite, valentinite, sernarmontite—occur sparingly in nature. Dry methods are generally adopted for the extraction of the metal. Electrometal-lurgical methods have had much attention in America and Germany and have not yet found, on economic grounds, practical or extended application, except in a few places. During recent years, treatment of the poor grades of the ore, especially sulphide, by ore-dressing methods, has commanded some attention and been adopted at a few plants. The impure sulphide of antimony, resulting from the liquation process, is called lLneedle," "liquated" or "crude" anti- mony, and the refined metal itself is called antimony "regulus." The different processes for the treatment of antimony ores are shown in the diagram of Fig. I. Liquation of Crude Antimony The first step in the smelting of antimony is a simple one, the process of LLliquation," which produces crude or needle antimony. Ores containing $ 50 per cent Sb are used in the liquation process for the production of crude. The temperature required for liquation is between 550' and 600°C. Ores to be liquated are broken to about walnut size. If the pieces are larger than this, the low heat used will not penetrate' effectively, and if they are smaller the ore tends to pack too closely for adequate penetration. A packed charge also prevents the free escape of the fused sulphide. Intermittent Liquation in Crucibles The unique type of furnace that is in use in China for smelting is not highly efficient but is simple in construction and operation. The furnace is generally built

Jan 1, 1944