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By J. W. Spretnak, H. R. Ogden, A. G. Imgram

The effect of working reduction, stress-relief annealing, and recrystallized grain size on the tensile and notch-tensile properties of molybdenum and Mo-0.5 Ti was studied. It was found that increasing the amount of working reduction increased the strength and reduced the tendencies toward brittle behavior. Stress -relief annealing did not alter the strength but lowered the transition temperature. Increasing the recrystallized grain size lowered the strength and raised the transition temperature. The notch -unnotch strength ratio began to decrease with decreasing temperature at temperatures below those at which the notched ductility fell to zero for all of the micro structural conditions investigated. BEING bcc metals, the refractory metals in Groups Va and VIa (V, Cb, Ta, and Cr, Mo, W) undergo a ductile-to-brittle transition and exhibit brittle fractures at low temperatures. Previous research has shown that molybdenum and tungsten not only have higher transition temperatures than columbium and tantalum but show a marked sensitivity of transition temperature to structure as well.' Recrystallized materials become brittle at considerably higher temperatures than is the case with material having a worked or fibered micro-structure. Evidence of structure sensitivity has also been detected in columbium- and tantalum-base alloys containing appreciable amounts of molybdenum or tungsten such as F-48 (Cb-15W-5Mo-1Zr) and Ta-10w.2 This paper describes the results of research conducted to further evaluate the effects of metal. lurgical structure on the low-temperature tensile and notch-tensile properties of molybdenum and Mo-0.5Ti. The effects of rolling reduction, stress-relief annealing temperature, and recrystallized grain size were studied. Considerable progress has been made in explaining the fundamental mechanisms of the flow and fracture characteristics of bcc metals. Several of these concepts are helpful in interpreting the data obtained in this study. Brittle fractures occur when the highly temperature-sensitive yield strength equals, or exceeds, the temperature-insensitive brittle cleavage fracture stress.3 The rapid increase in yield strength with decreasing temperature, characteristic of all bcc metals, is therefore of primary concern. petch4 has described the yield strength, ay, (stress required to initiate plastic flow) of bcc metals by the expression where ai is the frictional resistance to slip, Ky is a constant numerically equal to the slope of a a vs curve, and 2d is the average grain diamefer. The oi term itself is thought to be composed of a temperature-insensitive component dependent on impurity content and second-phase particles and a temperature-sensitive component dependent on the Pierls-Nabarro force.5 This equation has also been demonstrated to hold for the flow stress (stress required to maintain continued plastic flow).' Brittle-crack nucleation is thought to occur by the coalescence of dislocations piled up in slip planes at sessile dislocations or twin and grain boundaries.7,8 These proposed mechanisms require that a large number of dislocations be released into the active slip planes so that sufficiently large stress concentrations are produced at the dislocation pile-ups to enable coalescence into a micro-crack. Therefore, at least a microscopic amount of slip must occur in some grains to facilitate initial crack formation. Cottrell 7 has predicted that brittle fracture, nucleated by slip, should occur when where ty is the shear yield strength, ß = 1 in un- notched xension, u is the shear modulus, and y is the effective surface energy. This equation incorporates the Griffith concept of fracture that a crack will propagate if the decrease in strain energy equals or exceeds the increase in surface energy.

Jan 1, 1964

By B. W. Frazier

At a recent meeting of the North of England Institute of Min ing and Mechanical Engineers, during a discussion upon the com pression of air, attention was called to an apparent anomaly in the phenomena attending the compression. At a subsequent meeting this apparent anomaly was explained by Prof. Herschel, and all the facts observed shown to be strictly in accordance with the laws of thermodynamics. Upon reading the report of the discussion in the published transactions of the society, it occurred to me that an attempt to determine mathematically the amounts of energy (whether in the form of heat or of work) expended and absorbed in compressing air, and causing it to perform work by expansion, might prove of use to some who have not access to any treatise upon the application of the laws of thermodynamics to the compression of air, and who have not the time or the inclination to make such application for themselves. The apparent anomaly noticed was this: If air be compressed, and at the same time, by the sufficient application of a cooling medium, kept at a constant temperature, the indicator diagrams in the

Three. meetings for the presentation and discussion of papers were held in 1914, as follows: The 107th Meeting, including the Annual Business Meeting, in New York, Feb. 16 to 19; the 108th Meeting, Aug. 10 to 14, in Salt Lake City, and the 109th Meeting, Oct. 8 to 10, in Pittsburgh, Pa., under the auspices of Iron and Steel Committee, Committee on Coal and Coke, Committee on Petroleum and Gas, Committee on Non-Metallic Minerals. Local Sections ' Three new local sections were established during the year, namely; / Pennsylvania Anthracite Section, Chicago Section, and Utah Section.

Jan 1, 1917

By Gerald Greene

Tan various lead producers have given the subject of lead drosses much attention in recent years but the problem of their economical treatment is yet to be solved. Formerly the copper in the furnace feed was removed from the furnace in the form of matte. The speiss at that time consisted principally of the iron arsenide. The practice today is to roast off most of the sulfur and the copper in the feed forms a dross in the furnace, which is removed from the furnace with the lead. This material is poured into the drossing kettles and allowed to cool down to but slightly above the freezing point of lead. The copper dross, containing almost all of the arsenic and part of the antimony, is skimmed off and treated in a small reverberatory furnace at most plants. This is essentially a liquation process. The skimmed dross contains from 70 to 80 per cent lead, and much of this lead is liquated out. The products from this treatment are: (1) impure lead, (2) speiss and (3) matte. The speiss from the reverberatory furnace was studied in this research. The literature on the subject is of very little assistance, as almost no work has been done on the problem of establishing the exact identity of the various phases present. One author(1) states that speiss consists of a series of isomorphous compounds of the general formula FexAsy in which the Fe may be replaced by Ni, Co, Cu, Pb, Ag, Au, Pt, Zn, Cd and the As replaced by Sb, S and Bi. Hofman(2) states that the iron arsenide present is Fe5As.

Jan 1, 1935

By Edgar Shepard

THE interest of the Federal Government in improvement of water-ways dates from 1820, when Congress appropriated $5000 for making a survey of the Mississippi and Ohio Rivers and assigned this work to the Corps of Engineers of the Army. Since that time the Government has gradually assumed increasing jurisdiction in the matter of improvement and control of inland waterways until, by the River and Harbor Act of Jan. 21, 1927, Congress assigned to the Secretary of War and to the Chief of Engineers the duty of making surveys, in accordance with House Document No. 308, 69th Congress, to formulate plans for the most effective improvement of the navigable streams of the United States and their tributaries, for navigation, development of water power, control of floods, and the needs of irrigation. Virtually all the preliminary investi-gations and surveys required by this act have been completed. The reports made to Congress have been published and often are referred to as "308 Reports." The map shown in Fig. 1 is merely a skeleton distribution of the projects covered by these reports, but it serves to indicate the magnitude of the proposed undertaking. In many instances, a single character on the map stands for a major development involving several dams and reservoirs or many miles of canals or levees. The devastating floods of 1936, and the need for worthy public works to take up the slack in employment, gave further impetus to this program and in 1936 led to the enactment of a bill authorizing a large number of these projects.

Jan 1, 1940

By Paul Billingsley

THE term Boulder batholith was first applied in 1897 by W. H. Weed'2 to the extensive mass of granite in western Montana within whose borders occur the ore, deposits of Butte. In a general, way this was known to extend from Helena on the north to the Highland Mountains near Butte on the south, and to be relatively narrow in its east-west diameter. Its intrusive relations to the surrounding sedimentary , rocks, and its probable Tertiary age, were described by Weed, but in many ways his statements, based upon incomplete data, have required revision. Most notable of the errors of this description of the batholith were the failure,3 since corrected, to recognize the intrusive contact of the granite with the capping of andesite, and the complete absence of any reference to the many extensions of the granite beyond the somewhat narrow limits of its largest exposure.

Jan 1, 1915

By W. L. Phillips

Stress-strain data are reported for sodium chloride, lithium fluoride, and magnesium oxide tested in compression at diffevent strain rates in the telrlperature range from 70° to 873°K. Quantitative equations are given for the stvain-rate dependence of the critical resolved shear stress and the initial rate of work havdening. The properties so determined are compared with results previously reported for metals. ALTHOUGH the effects of strain rate and temperature on the stress-strain characteristics of metals have been extensively investigated1,2 these effects have not been studied in detail in ionic crystals. In the only previous investigations on the effect of strain rate on the deformation of ionic crystals. Gilman and gohnston3 and Hulse and pask4 have shown that the yield stress of lithium fluoride and magnesium oxide at room temperature is proportional to the ninth or tenth root of the strain rate. CRYSTAL PREPARATION Lithium fluoride, sodium chloride. and magnesium oxide single crystals were purchased from the Har-shaw Chemical Co. The compression fixture and sample preparation have been described in detail previously.5 The detectable impurities in MgO were eight parts in 105 of Fe and six parts in 105 of Si; in LiF, six parts in 105 of Mg; and in NaC1, two parts in 105 of Fe and four parts in 10&apos; of Mg. The cleaved samples measured - 0.1 in. by 0.1 in. by 0.3 in. Prior to testing all samples were annealed at -0.8 of their melting point and cooled to room tempera- ture at 50 C per hr.&apos; Samples were strained at rates (<) of 0.1, 0.01, 0.002, and 0.0002 in. per in. per min. EXPERIMENTAL RESULTS Fig. 1 is a plot of the critical resolved shear stress a,. (extrapolation of slope of easy glide region to zero strain) of sodium chloride, lithium fluoride, and magnesium oxide tested at different strain rates as a function of temperature. In all crystals at all strain rates a, decreases with increasing temperature according to an equation of the type397 where uo is a stress constant, K is a constant, and T is the absolute temperature. The points in Fig. 1 are the average of six tests. It is evident that there is a break in the log 0,- temperature plots at a characteristic temperature T,. The constant K of Eq. [I] is dependent on strain rate, Fig. 2. The relationship

Jan 1, 1962

By Charles L. Thomas

A novel, highly sensitive, and reproducible nzetlzod for the determination of hydrogen in solid materials is presented. The procedure requires equilibration of the specimen with hydrogen gas, rapid quenching, and hot vacuum extraction of the dissolved gas with subse-quent quantitative analysis by mass spectroscopy. Good linearity is obtained for the Arrl~enius plots of the investigated metals. The advantages in the use of this method over that of Sieverts aye discussed. The solubility data for copper are in reasonable agveewzent with a considerable number of other inuestigations, wllile those fov silver are considerably lower than previously reported. The first known solubility data for gold are presented. Solubility equations and heats of MUCH of the data which are available on the solubility of hydrogen in various metals and alloys have been obtained by the classical Sieverts method.&apos; The method involves the measurement of a decrease in pressure of a gas in a calibrated system, and the calculated contraction in volume is attributed to the solubility of the gas in the metal sample. The procedure requires several corrections, such as the solubility of the gas in the container walls and the diffusion of the gas through these walls, as noted by Steacie and .Johnson2 and others. In addition, errors may be incurred due to reactions between metal surface impurities, such as oxides, and the saturating gas. The precise calibration of the measuring system where large thermal gradients exist can present additional difficulties. Also, accurate volumetric measurements of small quantities of gas are difficult. Many of the objections to the Sieverts method were overcome on solid materials by Ransley and ~eufeld,~ who first saturated the metal with hydrogen and performed a subsequent extraction and measurement of the gas by chemical means. Eichenauer and pebler4 and Eichenauer, Kiinzig, and pebler5 measured the diffusion coefficient and solubility by following the degasification of a sample as a function of a rate of increase in pressure in a previously evacuated system. Here again, however, the procedure involves many of the corrections of the Sie-verts method. The present investigation deals with the solubility of hydrogen in solid copper, silver, and gold by a technique which eliminates many of the aforementioned corrections and possible errors. This procedure requires equilibration of the specimen with gas, rapid quenching, and hot vacuum extraction of the dissolved gas with subsequent quantitative analysis by mass spectroscopy. EXPERIMENTAL Two completely separate systems were employed to accomplish first, the equilibrium saturation of the sample and second, the extraction of the dissolved gas. Saturation Apparatus. The saturation apparatus, illustrated in Fig. l, consisted of a vertically mounted quartz tube with a three-way valve for vacuum or hydrogen near the top and an outlet near the bottom leading to a butyl phthalate seal. The bottom end of the tube was terminated with a joint accommodating an O-ring sealed "Asco Stirring Gland" (The Emil Greiner Co.). This gland facilitated movement of the thermocouple without introduction of air into the system. The upper portion of the tube (above the furnace) was water-jacketed. A Welsh 1405-B mechanical pump provided the necessary system evacu-

Jan 1, 1968

By H. I. Aaronson, C. Laird

Although the past results of X-ray experiments indicate that the broad faces of 0&apos; plates are coherent with their matrix, dislocations lying in arrays have frequently been observed at these boundaries by transmission electron microscopy. Critical experiments employing the latter technique have been carried out in order to determine the origin of these dislocations. It is concluded that 8&apos; plates are essentially coherent with the matrix at their broad faces throughout the aging temperature/time envelope studied. Virtually all of the dislocation arrays observed are deduced to have been formed by plastic deformation accompanying transformation. The proportion of dislocations arising from convexity of the plates is shown to be negligible by comparison with that from plastic deformation. At the higher aging temperatures, a[001] dislocations appeared in moderate numbers. These dislocations were traced directly, however, to the ledgewise dissolution of 0&apos; occasioned by the formation nearby of 0 crystals. On the other hand, since there is a parametric difference normal to the broad faces of the ?&apos; plates, mismatch dislocations do form at their edges. A previous conclusion that these dislocations have Burgers vectors of type a[001] was confirmed directly. The edges of 0&apos; plates were observed to develop octagonal shapes when growing, but circular shapes during dissolution. 1 HIS paper presents the results of an investigation of the interfacial structures of plates of the transitional phase, 8&apos;, formed in an A1-4 pct Cu alloy. In a companion paper, Part 11, the effects of these structures upon the migration kinetics of a:?f boundaries are reported. This work is pa.rt of a general program designed to establish the basis of precipitate morphology. The present authors in Al-Ag,1 and whitton2 previously in U-C alloys, have used transmission electron microscopy to examine directly the vander Merwe3-6 networks of dislocations anticipated7 to compensate the small amount of lattice misfit normally founda at the broad faces of Widmanstatten plates. Since the broad faces of 0&apos; plates are considered to be perfectly coherent with the corresponding habit planes in the a matrix,&apos; no dislocations should be present at these faces. Many reports have been published, however, giving evidence to the contrary.10-18 The primary objective of this investigation was therefore to ascertain the nature of these dislocation structures. An attempt to do this is described in the first three sections of this paper. Inspection of the matching of the a and 8 &apos; lattices at the orientations of the 0:0&apos; boundary corresponding to the edges of 0&apos; plates raises the possibility that these edges may be made up of rather closely spaced edge- type misfit dislocations oriented so as to be sessile with respect to the lengthening or shortening of the plates. Since this structure should severely inhibit migration of the plate edges (Ref. 7, Part II), a situation not originally anticipated,&apos; an experimental determination of the interfacial structure of the edges of 8&apos; plates was clearly in order, and is reported in Section III. Those aspects of the experimental procedure applicable to both Parts I and I1 are presented in the next section. Specific procedures applicable to individual aspects of each investigation, and also the relevant surveys of the literature, are then individually reported in the appropriate sections. I) GENERAL EXPERIMENTAL PROCEDURE The material used in both parts of these studies was the same as that of a previous investigation:" strips of A1-3.93 pct Cu, 0.009 in. thick, prepared as before, solution-annealed at 548°C for 6 hr, and quenched. Details of subsequent aging, and in some cases deformation treatments, are given in the Experimental Procedure sections of the individual parts of both papers. Specimens of the heat-treated strips were electro-thinned as beforeLg and examined in a Philips EM 200 microscope equipped with a goniometer stage. A commercial hot stage, of the grid-heater type and capable of * 30-deg tilt about one axis in the plane of the specimen, was also used for kinetic studies. The usual precaution of calibrating for the additional heat supplied by the electron beam was taken.19 A 16-mm cine cam-I era mounted outside the viewing window was frequently used to record the transformations. Conventional selected-area diffraction and dark-field viewing techniques were used to identify the precipitates in the foils. Normal bright-field images corresponding to two-beam diffracting conditions or dark-field images were employed to characterize the dislocations observed at the interfaces of the precipitates. The application of these techniques to the study of an interphase boundary, and the interpretation of the images,20&apos;21 has been fully described in a previous paper.&apos;

Jan 1, 1969

By G. L. F. Powell

g samples of Cu-20 wt pct Ag alloy have been mdercooled to a maximum of 197°C by melting under a slag of commercial soda-lime glass in a vitreous silica crucible. No grain refinement of the primary copper was observed in samples undercooled to the maximum of 197°C. When the samples contained a small amount of oxygen, the copper dendrites were partially recrystallized at undercoolings greater than 97°C. In previous papers&apos;-3 reporting the grain structure of undercooled silver and copper, it was observed that grain refinement was dependent on both undercooling and oxygen content. Grain refinement occurred in undercooled silver when the degree of undercooling exceeded the range 153" to 175"C, while in Ag-0 alloys (0.12 wt pct) fine equiaxed grains were exhibited when undercooling was greater than 50°C. Similarly, copper samples undercooled as much as 208°C displayed fan-shaped growth from a single nucleation site, while the grain structure of Cu-O alloys (0.08 wt pct) was fine and equiaxed at undercoolings larger than 150°C. Thus the presence of oxygen greatly reduced the undercooling at which grain refinement occurred. It was also observed that the change in grain size resulted from recrystallization and was not due to an enhanced nucleation rate in the liquid-solid transformation. It is possible that the influence of oxygen on recrystallization is due primarily to its presence as a solute element. walker4,&apos; reported that, although a grain size change did not occur in pure nickel until the undercooling exceeded 150°C, small grains were observed in samples of Ni-Cu alloy solidified at small and large degrees of undercooling. Jackson et al.6 suggested that the fine grained structure of the Ni-Cu alloy resulted from the melting off of dendrite arms during recalescence. This remelting process may occur in alloys as a result of segregation during freezing which causes a variation in liquidus temperature from point to point within a dendrite. It was therefore decided to undercool copper with a metallic alloying element to ascertain whether the presence of a metallic solute would have a similar effect to oxygen in inducing grain refinement. A Cu-Ag alloy was chosen, since both metals had been shown to behave similarly on undercooling. The alloy Cu-20 wt pct Ag was selected since the eutectic constituent outlines the initial growth form of the primary copper, so that the as-frozen grain structure is not obscured if subsequent recrystallization occurs. This paper describes the results of undercooling experiments carried out with Cu-20 pct Ag samples undercooled to a maximum of 197°C and the effect of oxygen content on the grain structure of the undercooled samples. EXPERIMENTAL Melting was carried out in a small cylindrical resistance furnace using "fine" silver granulate and oxygen-free high conductivity copper. The procedure adopted was to melt the required quantity of silver in air in a clean vitreous silica crucible for approximately 15 min, freeze, and add granulated commercial soda-lime glass to form a complete surface slag cover, after which the sample was melted and frozen several times to reduce the oxygen content. The glass slag cover was approximately 3 in. thick. Pieces of copper (=50 g) were added to the crucible until the required quantity to make 350-g samples of alloy had been charged. Each piece was added quickly to the crucible which was held at a temperature slightly above the melting point of silver. The piece was quickly pushed beneath the glass to minimize oxidation and any oxide coating usually decomposed before the piece had settled down into the silver. After the full quantity of copper had been added, the melt was stirred with a silica rod to hasten homogenization and a Pt/Pt 13 pct Rh thermocouple enclosed in a vitreous silica sheath inserted for temperature measurement. Heating and cooling curves were recorded on a potentiometric chart recorder fitted with a zero suppression unit. The milli-voltage range of the recorder was adjusted so that temperatures could be read to 1°C. Heating and cooling curves were taken every hour until three consecutive readings gave the same solidus-liquidus range, consistent with the solidus-liquidus range for this alloy composition by reference to Hansen and Anderko.7 Metallographic examination of samples frozen at this stage, failed to show any variation in composition from bottom to top of the ingot. Consequently, it was considered that the melt was homogeneous at this stage and undercooling experiments were then car-

Jan 1, 1970

By John T. Norton

N order to attempt to arrive at a better under-Jl standing of the whole basic problem of sintering, these remarks will serve as an introduction for discussion that is included and will, perhaps, help to isolate specific questions which need to be answered or to suggest some definite avenues of investigation which should be followed. To bring some sort of logical order into the presentation, I will consider the various types of interaction between the metal to be sintered and the atmosphere which surrounds it, depending upon whether the phenomena are essentially chemical or physical in nature. For example, when the only necessary criterion for the satisfactory sintering of a certain powder is the removal of an oxide skin, then the problem of choosing a suitable atmosphere is primarily chemical; however, if a special surface condition as a consequence of the oxide skin removal is necessary for particularly effective sintering, then the problem becomes a physical one. Of course, the two aspects overlap considerably, but it may be possible to make a distinction in principle if not in practice. The chemical characteristics of the phenomena will be emphasized, since these are the better known. Metal-gas reactions involved in sintering are controlled primarily by the thermodynamics of the processes involved. In which direction will a reaction go and how far before it stops? The answer is to be found in the magnitude of the free energy change associated with the reaction. If a constituent is to be removed from the specimen as completely as possible or if a constituent is to be formed in the specimen as completely as possible, then one chooses conditions which are far from equilibrium so that the reaction is driven toward completion. On the other hand, if the composition is to be maintained at a desired value, then conditions are adjusted as closely as possible to the equilibrium point. This aspect of the problem is susceptible to quite precise analysis, provided, of course, that the significant reactions can be recognized and the required thermodynamic data are available. Conversely, if one asks how fast the reaction goes or how far it proceeds in a given time, the answer is frequently much more difficult to answer in quantitative terms. Yet the rate-con trolling factors of the reactions may be of primary importance in the success of a particular operation, especially where competing processes are at work. Both equilibrium and rate factors must be understood if a clear picture is to be obtained. For instance, in a process for carburizing titanium dioxide, is the difficulty of obtaining a stoichiometric Tic due to a true limitation of the equilibrium or simply to a very slow rate of reaction? An example of this appears in the work of Kalish and Mazza.&apos; They showed that the oxygen content of sintered iron compacts was lower when sintered in pure hydrogen than in the case where the hydrogen was diluted with either argon or nitrogen. The equilibrium oxygen content of the iron would be the same in the two cases, since it is determined by the ratio of the partial pressures of water vapor and hydrogen and this pressure ratio is unchanged by dilution. The rate of oxygen removal, however, under the conditions of a constantly replaced furnace atmosphere, depends upon diffusion and thus upon the concentration of hydrogen in the furnace atmosphere. Possibly the clearest way to illustrate the interplay of these two factors is to consider in more detail some of the typical metal-gas reactions. Adsorbed Gases It is common experience that fine metal powders with their very large surface areas often contain large quantities of gas. This gas, which results from exposure to air or perhaps from some step in the

Jan 1, 1957

By R. W. Heckel, R. E. Trabocco

The recovery process in 400 Monel filings was followed, principally, by using the Warren-Averbach technique of X-ray peak profile analysis. The deformation fault probability, a, was 0.006 in samples of unannealed filings. a , the twin fault Probability , was approximately 0.002 in samples of unannealed filings. Both a and 0 were found to "anneal out" at 600°F. The effective particle size and mzs strain increased and decreased in the (111) direction, respectively, with increasing annealing temperature. The actual particle size was found to be almost equivalent to the effective particle size. Tile small values of deformation and twin fault probabilities accounted for the similarity in values of the effective and actual particle sizes. Stored strain energy and dislocation density calculations based on rms strain decreased with increasing annealing temperature. The dislocation density decreased from 10" per sq cm in the unannealed filings to 10&apos; per sq cm in the partially re-crystallized filings. The square root of the dislocation density based on strain to that based on particle size indicated a random dislocation distribution in the unannealed filings. The dislocation arrangement changed to one with dislocations in cell walls with increasing annealing temperature. THE recovery processes which occur in metals are generally thought to be a redistribution and/or annihilation of defects.&apos; Investigators&apos; have shown that recovery processes can be characterized by X-ray line-broadening analyses. Michell and Haig4 measured the stored energy of nickel powder by calori-metry and found the value to be greater by a factor of 2.5 than that from X-ray data obtained by the Warren-Averbach technique.= Minor increases in particle size occurred up to 752°F (recovery), while above 752°F the particle size increased greatly due to recrystalliza-tion. X-ray microstrain values decreased between room temperature and 392"F, remained constant from 392" to 752"F, and decreased from 752°F to a negligible value at 1112°F. Faulkner developed an equation for calculating stored strain energy based on X-ray line-broadening data which gave a closer correlation of measured and calculated stored strain energy based on the data of Michell and Haig. The stored strain energy released during recovery is predominately dependent on the decrease in dislocation density which was p-enerated from cold work.7 Stored energy has been measured8 in alkali halides during recovery and recrystallization and 80 pct of the stored energy was found to be released during recovery. Dislocation distributions have been studiedg in a number of fcc metals by thin-film electron microscopy. Howie and Swann" found the stacking fault energy of copper and nickel to be 40 and 150 ergs per sq cm, respectively. ~rown" has pointed out that these stacking fault energy values should be corrected to 92 and 345 ergs per sq cm, respectively. The dislocation distribution of a metal is directly dependent on the stacking fault energy of the system. Metals of high stacking fault energy such as aluminum cross-slip readily and do not form planar arrays of dislocations. Metals of lower stacking fault energy such as stainless steels" do not cross-slip readily. Cold-worked nickel has been found to form a cellular dislocation structure after annealing.13 The relatively high stacking fault energy of nickel and copperlo to a lesser extent favor cellular structures of dislocations rather than planar arrays after deformation. The present study of recovery was carried out on a Ni-Cu alloy (Monel 400) to compare with prior studies for pure nickel and pure copper. X-ray line-broadening techniques were used to measure the effect of recovery temperature on rms strain and particle size and the results were compared with previous studies on copper&apos;4-&apos;7 and nickel., Calculations were also made on stacking fault probabilities, dislocation density, dislocation distribution, and stored strain energy as affected by temperature. EXPERIMENTAL PROCEDURE The nominal analysis of the Monel 400 used in this investigation was: 66.0 pct Ni, 31.5 pct Cu, 0.12 pct C, 0.90 pct Mn, 1.35 pct Fe, 0.005 pct S, 0.15 pct Si. The annealed material was cold-reduced in two batches, one 50 pct and the other 80 pct. It was originally planned to conduct line-broadening studies of these bulk samples; however, rolling textures that developed produced low-intensity peaks which were not suitable for line-broadening analysis. Filings were prepared at room temperature from both the 50 and 80 pct cold-reduced specimens, series A and series B, respectively, and were not screened prior to heat treatment or X-ray studies. Heating to the annealing temperature, 200" to 120O°F, was accomplished in a matter of minutes in a hydrogen atmosphere. Following heat treatment, some of the filings were mounted and polished for microhardness measurements with a Bergsman microhardness tester, using a 10-g load. A G.E. XRD-5 diffractometer using nickel-filtered Cum radiation was used to obtain all diffraction patterns. Only (111)- (222) line-broadenin data were used in the present study since the {400f peaks were too weak to use. The Fourier analysis of the (111) and (222) peak

Jan 1, 1969

Theo. B. ComstocK, Los Angeles, Cal. (communication to the Secretary*):—Mr. Blake&apos;s recent paper upon this topic undoubtedly partly explains the rationale of a part of the known facts bearing upon discolorat&apos;ion and encrustation of rocks. His quotation from Humboldt, with reference to certain South American examples, may be questioned in the light of further facts, which do not appear to bear out the great traveler&apos;s theory of causation. There is no available evidence that the waters of the tropical rivers referred to by Professor Blake contain dissolved organic matter in the varying proportions required to demonstrate Humboldt&apos;s guess, nor do the concomitant facts in any manner bear out the hypothesis that the blackening in one case and its absence in the other may, perhaps, be traced to differences in the chemical reactions of the respective waters. Careful consideration of Professor Blake&apos;s illustrations, in connection with numerous personal observations extending over widely-scattered areas, convinces me that elements of

Jan 1, 1905

By Charles Wurms, Robert Steinitz

DURING an investigation to determine the compatibility of several metals with tungsten, the degree of reaction between tungsten and lead was determined. A literature survey showed considerable disagreement between the results of various earlier investigators. Information presented by M. Hansen1 states that, according to S. Inouye,2 tungsten has very poor resistance against attack by molten lead, even at the low temperature near the melting point of lead. A phase diagram in the same reference indicates a solubility of 30 wt pct W in molten lead at 1300°C. Contrary evidence was shown by Parkman and shepard3 in their investigation of materials for use in heat transfer systems containing liquid lead alloys; they performed experiments at 980°C for times up to 50 hr without noticing any appreciable attack on the tungsten. Tungsten sheet was immersed in molten lead contained in Vycor tubes evacuated to at least 10-4 mm Hg. R. Bernard4 and R. I. Jaffee5 also indicate that no reaction occurs between molten lead and tungsten. However, no experimental data were included in these reports. In order to settle the question of the solubility of tungsten in molten lead, tungsten powder with an average Fisher subsieve particle size of 6µ was pressed in a double-acting die at 6 tsi to small compacts. They were then sintered in an atmosphere of hydrogen for 2 hr at 1700°C, resulting in a sintered density of 64 pct of theoretical with final dimensions of 0.260 in. in height and 0.245 in. in diameter. For all tests, the tungsten pellets were immersed in molten lead. Table I is a summary of the experimental procedures showing atmospheres, temperatures, and times. The first experiments were performed at 650°C; at this temperature, the liquid lead should wet the porous tungsten better than at its melting point, and penetrate into the pores. The lead was heated in a graphite crucible with a graphite cover. No protective atmosphere was used, as it was expected that the formation of CO would be sufficient to prevent oxidation. This, however, proved to be wrong, and all tungsten samples showed a slight oxide film after treatment. The tungsten samples were immersed in the molten lead for times of 5 min, 10 min, 1/2 hr, 1 hr, and 2 hr. After this time, the melt was poured into a form and the

Jan 1, 1962

By J. S. Ll. Leach, M. B. Bever

THE system copper-nickel exhibits complete solid and liquid miscibility1 The thermodynamic properties of such a system would not be expected to deviate greatly from ideality. Although the evidence is conflicting, anomalies in the composition dependence of various physical properties of solid copper-nickel alloys suggest that mixing may not be ideal.&apos; From measurements of the Hall coefficient it has been concluded that clustering occurs in these alloys. &apos; Considerations involving the phase diagram of the ternary system copper-nickel-chromium have led Mei-jering3 to predict a positive heat of formation for solid copper-nickel alloys. An electrochemical investigation of the activity of nickel in copper-nickel alloys showed unexpectedly large positive deviations from ideality.4 wagner5 has proposed that if the entropy can be considered ideal, these measurements would yield the following equation for the heat of mixing at 700°C H" = 3380 x,vl (l-xVi) cal per g atom [I1 The heat of formation at 722°C of solid copper-nickel alloys of the equiatomic composition has been measured in a reaction calorimeter as 540 cal per g atom. This note reports calorimetric measurements of the heat effects on dissolution of some copper-nickel ndon: in tin. These measurements were preliminary to a larger investigation, which was later discontinued. From them the heats of formation of the alloys can be calculated, if certain assumptions are

Jan 1, 1960

By J. S. Kirkaldy, G. R. Purdy

THE formation of ferrite in supersaturated aus-tenite has been the subject of considerable speculation and investigation. Aaronson has recently reviewed the data pertinent to this reaction.&apos; Since these data in all cases refer to ternary or high-order alloys it is not possible to put them to the test of simple binary diffusion formalism. It has not, therefore, been possible to make a certain statement as to the controlling mechanisms in the process. An assessment of the difficulties inherent in the conventional statistical metallographic approach suggested that a study of the problem by means of a macroscopic two-phase diffusion couple might contribute useful information. Accordingly, such a couple was synthesized, and the rate of motion of a ferrite-austenite phase boundary (the growth of an austenite layer at the expense of a ferrite layer) was determined. Wagner originally produced a diffusion solution applicable to the motion of a planar phase interface in a binary diffusion couple, assuming local equilibrium throughout the diffusion zone. This solution, which is stated free of typographical error* in Ref. where a is the position of the interface in A space (A = x/fi), C; and CL1 are the equilibrium inter-facial concentrations in phases I and 11, C: and C*1 are the initial bulk concentrations in phases I and 11, and & and are diffusion coefficients (assumed constant). If a diffusion couple consisting of homogeneous layers of ferrite and austenite in equilibrium is raised to a higher temperature, the austenite layer will grow at the expense of the ferrite. Provided that the thickness of the ferrite layer is much less than the diffusion length of carbon in ferrite, we can set , so that Wagner&apos;s solution reduces to

Jan 1, 1963

By C. L. Sollenbeger, R. B. Greenwalt

PERHAPS the most widely used dispersants or gangue depressants in nonmetallic flotation are sodium silicates, which vary in silica-to-soda ratio from 1 to 3.75. Typical manufactured silicates in order of decreasing solubility and increasing amounts of silica are Metso, silica-to-soda ratio of 1.00; D, 2.00; RU, 2.40; K, 2.90; N, 3.22; and S-35, 3.75.* References in flotation literature1,2 to the use of sodium silicates are often weak because they fail to mention the type of silicate used. Metso and silicate N have occasionally been mentioned, but when the type of silicate is not mentioned, it is usually assumed to be N, the cheapest of the soluble silicates and the one recommended by sodium silicate manufacturers as a flotation agent. In the All is-Chalmers Research Laboratories a systematic study was made of the effect of different alkali-silica ratios on the concentration by flotation of two scheelite ores. One of these was a high grade ore from the Sang Dong mine in Korea. The effect of such factors as pH; addition agents; and conditioning time, temperature, and pulp density on the flotation efficiency of this ore have been described previously. The other ore was a low grade ore from Getchell Mines Inc., Nevada. The mineralogy and techniques of concentrating this ore have been described by Kunze. Hereafter these ores will be referred to as the Korean and Nevada ores. Experiments were made with both to determine the effect of three factors—-type of silicate, concentration of silicate, and pH of the pulp—on recovery and grade of tungsten in a rougher concentrate. Average WO, content of the Korean ore was 1.50 pct and of the Nevada ore 0.27 pct. The predominant tungsten mineral in both ores was scheelite, which was accompanied by a small amount of powellite. The powellite and scheelite were finely disseminated through both ores and required a —200 mesh grind for liberation. Major gangue minerals in the Korean ore, in decreasing order of abundance, were amphi-boles, quartz, biotite, garnet, fluorite, and calcite. Bulk sulfides composed about 3 pct of the total weight. Gangue in the Nevada ore, in descending order of abundance, was garnet, alpha quartz, calcite, phlogopite, wollastonite, and amphiboles. Sulfide minerals were 3 to 4 pct of total weight. Batch flotation experiments were made with 500-g samples of ore, each sample wet-ground to 90 pct passing 200 mesh. The finely ground ore was floated in a Fagergren batch cell at 25 pct solids. The natural pH of the Nevada ore was 8.9 and of the Korean ore, 8.5. The D, RU, K, N, and S-35 sodium silicates were obtained in colloidal dispersions with varying amounts of water. The most alkaline, Metso, was in dry powdered form. For convenience in addition, 5 pct solutions by weight were prepared from each of the silicates, on the basis of dry sodium silicate dissolved in the correct amount of distilled water. Chemical analyses of the various silicates are given in Table I, together with the pH of the 5 pct solutions. A preliminary bulk sulfide float was made with secondary butyl xanthate as the collector and pine oil as the frother. The WO] analysis of the sulfide concentrate was nearly 1 pct for the Korean ore and about 0.1 pct for the Nevada ore. The tungsten contained in the sulfide concentrate constituted about 3 pct of the total tungsten in each ore. No effort was made to recover these tungsten values. The scheelite was floated with oleic acid. Adjustments in pH were made with sulfuric acid or sodium carbonate. A 1 pct solution of 85 pct Aerosol OT was sprayed on the froth and sides of the cell during the scheelite float to aid in dispersing the minerals and to decrease the entrapment of gangue particles. Six tests were planned for each of the six types of silicate in which concentrations of 1, 2, and 4 1b of silicate per ton of dry ore were investigated at both 6.5 and 10 pH. All tests were made at room temperature. The performance of each silicate was judged from the grade and recovery of WO, in the scheelite rougher concentrate. Tungsten recovery was calculated on the basis of the scheelite remaining in the ore after the preliminary sulfide float. Testing of each silicate at three levels of concentration and two levels of pH required 36 tests with each scheelite ore. Variance analyses were performed on the concentrate grades and recoveries to determine whether or not the type of sodium silicate, the concentration of sodium silicate, or the pH significantly affected recovery or grade. Results Concentrate Grade: A variance analysis of the concentrate grades for the Korean ore showed that concentration of the silicate and pH of the ore pulp were major factors in producing a high grade concentrate. Also, the silica- to-so da ratio was important as an interaction with pH. The concentrate grade vs silica-to-soda ratio is plotted in Fig. 1. The curves show that the concentrate grade improved with an increase in concentration of sodium silicate and also

Jan 1, 1959

By Rudolf Gahl

Page Tests Conducted in Small Test Mill................... 577 Demonstration Tests Conducted by Minerals Separation Co....... 577 Flotation Tcsts Conducted by Inspiration Co............. 577 Sampling of Orebody........................ 578 Other Results Obtained in Small Test Mill.............. 580 Tests Conducted in Large Test Mill................... 580 Flow Sheet............................. 580 Discussion of the Value of Preliminary Table Treatment......582 Callow Flotation Installation..................... 585 Flinn-Towne ~nstallation...................... 587 Cole-Bergman Installation...................... 588 Methods Followed in Competitive Tests................ 590 Advantage of Pneumatic Flotation Machines.............. 591 Pneumatic Machines of Minerals Separation Co............. 591 Float Skimming Device......................; 594 Experimental Inspiration Flotation Machine.............. 596 Arrangement of Callow Cells in Series ................ 598 Variations of Flow Sheet....................... 599 Coal Tar as Flotation Agent..................... 600 Experience with Primary Slime.................... 602 Influence of Iron on Flotation..................... 605 Influence of Chemicals on Primary Slime............... 607 Fineness of Crushing Desired.................... 607 Operation of Large Concentrator..................... 608 Flow Sheet of Callow Sections.................... 608 Flow Sheet of Inspiration Sections.................• 609 Inspiration Flotation Machine of Steel Construction.......... 610 Minerals Separation Section..................... 613 Filter Plant............................ 613 Results Obtained in Commercial Concentrator............... 616 Tonnage............................... 616 Air and Power Consumption...................... 616 Floor Space............................ 617 Water Consumption......................... 617 Recovery............................. 618 Oil Consumption.......................... 618 Operating Costs for Flotation..................... 620 Discussion of Results Obtained.................... 620 Prospects for Futurc Development of the Flotation Process......... 621 Porous-Bottom Experiments..................... 622 Raising the Grade of Concentrates.................. 624 Recovering Carbonates by Flotation................. 624 Recovery of Silicates by Flotation.................. 627 General Theory......................... 628 Conclusion............................... 630

Jan 1, 1917

By E. A. G. Colls

Discusses corrosion in Trail chemical plants producing ammonia, sulphuric, nitric and phosphoric acids, ammonium phosphates, sulphate and nitrate, together with miscellaneous allied material problems and their solution using erosion or corrosion proof materials. Conclusion, that for work of this nature, most costly material may well be cheapest in the long run.

Jan 4, 1950

By Jr. Ensign C. O., J. W. Trammell

The two principal methods of room-and-pillar mining practiced at White Pine make it important to predict variations in the thickness and rock types of a stratum called the upper sandstone. In full column mining, the nearly barren upper sandstone occurs between two ore horizons (called upper shale and parting shale, respectively), and is mined as a part of the ore column. In general, full column mining is not practiced where excessive upper sandstone thickness causes full column ore grade to be substantially lower than parting shale ore. In parting shale mining, the upper sandstone forms the mine roof. Difficulty in predicting upper sandstone character arose because the extent and directions of its variations were not apparent in the property&apos;s diamond drilling, in which holes are spaced on 1000-ft centers. A study of sedimentary features, undertaken to improve the predictability of trends in the upper sandstone, led to an interpretation of the sedimentary environment in which the sandstone was deposited. Ripple marks, mud cracks, and cross-bedding, as well as other, less well known features, such as channel casts, flute casts, and current crescent casts, were mapped or recorded. These data, coupled with the knowledge of regional facies changes gained from studying drill core, show that the upper sandstone was deposited by a series of streams flowing northeastward over the underlying parting shale. Deposition of the lowermost bed of the upper sandstone, near the ancient shoreline, was locally preceded by erosion of the parting shale, and the greatest thicknesses of sandstone are found in channels scoured out of the parting shale. Awareness of the rather strong linear trends in the upper sandstone makes it possible to project continuous areas of thick upper sandstone through apparently isolated "highs" in the upper sandstone thickness contour map, which is based on drill-hole information. Since local exceptions to general stratigraphic trends exist, a method was also needed for esti- mating, in detail, the thickness and degree of shali-ness of upper sandstone forming the roof in active parting shale mining areas. Because locally the parting shale was thinned by erosion during the deposition of upper sandstone, parting shale thickness is inversely proportional to upper sandstone thickness. Utilizing information taken from short drill holes into the roof, curves were constructed for the correlation of parting shale thickness (measurable in the mine) with the upper sandstone total thickness, as well as the thickness of its basal member. The White Pine mine is situated in Ontonagon County, approximately 6 miles south of Lake Superior, in the Upper Peninsula of Michigan (Fig. 1). The orebody mined by White Pine Copper Co. occurs in the lowermost 20 to 25 ft of the Nonesuch formation, a series of middle- to upper-Keweenawan shales, siltstones, and sandstones. This paper discusses the solution of problems in ore grade control and mine planning arising from the presence of an essentially barren sandstone stratum within the orebody. THE OREBODY AND MINING TYPES A brief description of the orebody and mining methods is necessary to show how the upper sandstone affects mine planning and grade control. In the mine, the cupriferous zone of the Nonesuch shale is divided into three major portions, as shown in Fig. 2. Lying conformably on top of the Copper Harbor formation (or "lower sandstone") is the lower part of the orebody, the parting shale. The parting shale is overlain by the upper sandstone. On top of the upper sandstone, the basal portion (8 ft) of the upper shale is quite similar to the parting shale. Both the upper shale and parting shale are divided into a number of smaller stratigraphic units, each having a characteristic copper content, as shown by the histogram of Fig. 2. Other authors1&apos;3 have dealt in detail with the stratigraphy and mineralogy of the orebody. However, in this article, we are concerned with the major subdivisions only, and it will suffice to note the low copper content of the upper sandstone, shown in Fig. 2. At present, two types of room-and-pillar openings are created in the orebody. In one type, called parting

Jan 1, 1964