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By P. Shahinian, H. H. Smith, M. R. Achter

Crack growth rates are measured at elevated temperature in a resonant fatigue machine from vibration frequency decreases calibrated in terms of crack depth. Crack growth rates in Type 316 stainless steel at 500º and 800°C show a sharp increase with oxygen pressure in an intermediate pressure range and little or no change at high and low pressures. At 500°c, I torr of oxygen reduces the fatigue life by almost a factor of 100 in comparison to that in vacuum and raises the growth rate of shallow cracks by the same At At 800°C the effects are smaller. Changes in slope in the crack growth rate curves are discussed in terms of a model in which rates of surface production and of surface coverage by gas are compared. The use of a calculation method in which the surface exposure time is equal to X/v, where x is the interatomic spacing and v is the growth rate, makes it possible to obtain order of magnitude agreement at 500°C between the observed pressure and the predicted pressure at these slope changes. At 800°C oxidation becomes a .factor and the data cannot be treated by simple adsorption theory. THE decrease in the fatigue life of metals as a function of gas pressure usually follows a stepped curve with virtually all of the decrease concentrated in a sharp drop in a transition zone at intermediate pressures and little or no change at low and high ranges. A number of models, differing in the details of the mechanism, have been offered to explain the shape of the curve. Measurements of crack growth in aluminum as a function of gas pressure by Bradshaw and Wheeler' and Hordon2 demonstrated opportunities for quantitative comparison to evaluate the proposed models. Since comparable data were lacking at high temperatures, in the present work rates of crack propagation were measured in Type 316 stainless steel at 500" and 800°C as a function of oxygen pressure. Choice of this material was dictated by two considerations; it is stiff enough at these elevated temperatures to resonate with the regenerative drive on our fatigue machine and it is known to display a large effect of environment. A new method of calculation is described to predict the gas pressure at the critical point. EXPERIMENTAL PROCEDURE Because of the difficulty of measuring crack depths directly at high temperatures, an indirect method was developed based on the decrease in the resonant frequency with the growth of a crack. A reversed bending, constant amplitude fatigue machine, described previously,3 vibrates a specimen at its resonant frequency, automatically records any changes in it and shuts itself off after it has reached a preset value of frequency decrease. The record of frequency change is used to determine the rate of crack growth. Sheet type specimens of Type 316 stainless steel, Fig. 1, incorporated a sharp, shallow notch to localize the formation of a single crack. After machining, they were annealed in a vacuum of l0-6 torr either at 1066" (lot A) or 871°C (lot B) and then electropolished in an acetic-chromic acid solution. Bending strains were measured at 500" and 800°C by an optical technique4 and reported as total strain without correction for the notch. At 500°C, the 0.141 pct strain was 0.085 pct elastic and the remainder plastic. At 800°C the 0.062 pct strain was all elastic. To convert frequency decrease to crack length, calibration curves were obtained by interrupting the vibration at stated intervals of frequency decrease. The crack depth was measured microscopically at a magnification of X400 and reported as the average of the measurement on each edge. Some specimens were sectioned for crack measurement while others were returned to the machine and fatigued further. There was good agreement between the two methods. Before beginning the vibration, the vacuum chamber was first evacuated cold to 1 x 1O-6 torr, then heated to the operating temperature and held there until the pressure was again reduced to 1 x10-6 torr at which time oxygen was introduced to the desired pressure. In this investigation the vibration frequency was nominally 10 cps and a decrease of 0.6 cps was taken as the failure point. The choice of the frequency decrease to represent failure has no appreciable effect on the fatigue life because the crack is growing very fast at this point.

Jan 1, 1970

By D. V. Edmonds, C. J. Beevers

Tensile tests were carried out on a! titanium containing 850, 1250, and 2700 ppm 0, and up to -500 ppm H. The tests were performed at -196", -78", 20°, 150°, and 300°C at a strain rate of -1.0 x 10??3 sec-1. Increasing oxygen content, increasing grain size, and decreasing test temperature resulted in enhanced embrittlement of the a titanium by the hydrogen additions. Metallographic observations showed that this can be correlated with the influence of these parameters on the introduction of cracks into the a! titanium by fracture of titanium hydride precipitates. CRAIGHEAD et al.1 reported that the hydrogen content normally found in commercial-purity a! titanium (60 to 100 ppm) was sufficient to cause a substantial lowering of the impact strength, and they attributed this embrittling effect of hydrogen to the precipitation of titanium hydride. Lenning et al.&apos; found that in commercial-purity a titanium there is an almost complete loss of impact strength at about 200 pprn H, which is approximately half the value needed to eliminate the impact strength of high-purity a titanium. They also showed that the presence of 3000 ppm hydrogen reduces the room-temperature tensile ductility of commercial-purity material to a value of the order of 10 pct; the corresponding hydrogen concentration for high-purity titanium is over 9000 ppm. It thus appears that the detrimental effect of hydrogen on the mechanical properties of commercial-purity titanium becomes evident at much lower hydrogen contents than for high-purity titanium. The main difference between the two types of a titanium might be expected to be the higher level of interstitial impurity in the commercial-purity grade. Jaffee et a1.3 studied the influence of temperature and strain rate on the hydrogen embrittlement of high-purity and commercial-purity ! titanium. In general, the behavior was the same for both materials; embrittlement was enhanced by decreasing temperature and increasing strain rate. Recent results from tests on commercial-purity a titanium containing 850 ppm O and varying amounts of hydrogen up to -500 ppm showed that the degree of embrittlement by hydrogen is intimately related to the fracture characteristics of titanium hydride precipitates.4 The present paper considers the interrelationship between the mechanical properties and micro-structural features of commercial-purity a! titanium containing 850, 1250, and 2700 ppm 0 and varying amounts of hydrogen up to -500 ppm. 1. EXPERIMENTAL PROCEDURE Three types of commercial-purity titanium supplied by IMI* were used in the investigation, and for the *Address: Witton, Birmingham 6, United Kingdom. purpose of this paper are designated Ti 115, Ti 130, and Ti 160. The principal impurity elements are given in Table I. The material was received in the form of 12.7 mm diam bars having a fully recrystallized structure. Tensile specimens with a round cross-section of 4.5 mm diam and a gage length of 15.2 mm were machined from the bars. In order to develop the same grain size (mean linear intercept of grain boundaries) in each of the three types the specimens were annealed under a dynamic vacuum of <10?5 mm Hg, Table 11. Specimen hydriding was carried out in a modified Sieverts apparatus;&apos; hydrogen was taken into solution at 450°C and after holding the specimens at this temperature for 24 hr they were furnace-cooled to room temperature at an average rate of -100 C deg per hr. By this method nominal hydrogen contents of 0, 50, 100, 250, and 500 ppm were introduced into specimens of Ti 115, Ti 130, and Ti 160 (100 ppm (wt) -0.5 at. pct). The actual hydrogen contents were calculated from the weight differences obtained by weighing the specimens before and after the hydriding treatment. Tensile tests were carried out at temperatures of -196", -78", 20°, 150°, and 300°C on a 10,000 kg In-stron machine at a nominal strain rate of -1.0 x 10-3 sec-1. Fractured specimens were sectioned in planes parallel to the tensile axis, mechanically polished to 0.25 µm grade of diamond paste, and then attack polished using a solution containing by volume 99 parts H2O, 1 part HF, and 1 part HNO3. Although the latter treatment unavoidably opened out cracks and voids visible after mechanical polishing, it did reveal the grain structure, titanium hydride morphology, and deformation twinning structure.

Jan 1, 1970

By J. J. K. Daemen, C. Fairhurst

Introduction The stress field around a supported tunnel can be considered as being composed of: i) the virgin (pre-mining) stress in the rock ii) the (elastic) change in this stress field caused by creating the opening iii) the (time-dependent ) change in the stress field produced by (i) and (ii) as a section of the rock breaks up iv) the (time-dependent) influence of the stress build-up in the support. Several authors have examined the conditions necessary to produce static equilibrium between the support, the rock, and the regional (in-situ) stress field. The analysis used by Labasse (1) is typical. Consider a circular tunnel radius R in a hydrostatic stress field (P), and a radial pressure pi exerted by the support. According to Labasse, the radius ‘b’ to which the rock will break* for a given support pressure, pi, can be calculated from: - the equilibrium equation: [ ] As a zone of broken rock develops around the opening, the stress circle for a point on the elastic-broken rock boundary moves to the right in the Mohr diagram until the radial stress in the broken zone s equal to the radial stress in the elastic zone.

Jan 1, 1971

By E. J. Rapperport, E. D. Levine

The boundaries of the (a +ß) field in the Al-Li system were determined between 150°and 550°C utilizing quantitative metallography and lattice-parameter measurements. The solubility of lithium in aluminum decreases from 12.0at. pct Li at 550°C to 5.5 at. pct Li at 150°C. P Al-Li is saturated with aluminum at 45.8 at. pct Li and has this boundary value constant over the temperature range 150°to 550°C. THE solid solubility of lithium in aluminum has been determined by several investigators, 1-6 but, as shown in Fig. 1, there is little agreement among the various determinations. The earliest investiga-tions&apos;-&apos; are suspect because of the use of impure materials. Although high-purity materials were employed in more recent work,4&apos;5 the experimental techniques may have led to contamination of the specimens. Probably the best work has been that of Costas and Marshall,6 who obtained close agreement between results obtained by two independent phase-boundary techniques: electrical resistivity and mi-crohardness. No detailed studies of the solubility of aluminum in the bcc ß phase, Al-Li, have been reported. Cursory investigations1,2,6 have indicated only that the (a+ß) -p boundary lies between 40 and 50 at. pct Li and is relatively independent of temperature. The present work was undertaken in order to provide an independent check on Costas and Marshall&apos;s determination of the solubility of lithium in aluminum, to extend knowledge of this solubility limit to temperatures below 225°C, and to make an accurate determination of the solubility of aluminum in Al-Li. EXPEFUMENTAL Alloy Preparation. In view of the difficulties encountered in previous investigations of the A1-Li system, close attention was paid to the use of methods of alloy preparation and treatment that would minimize contamination. Aluminum sheet (99.99 + pct Al) was vacuum-induction melted in a beryllia crucible to remove hydrogen. Lithium (99.9 pct Li) was charged with pre-melted aluminum into a beryllia crucible, in a helium-filled drybox. The crucible was sealed in a Vycor tube and transferred from the drybox to an induction furnace. Melting of alloys was performed by induction heating in a helium atmosphere. Solidification was accomplished by means of a suction apparatus, shown in Fig. 2, in which the alloy was forced by changes of pressure into a 3/16-in. inside diam closed-end beryllia tube. This technique produced rapid solidification of a small portion of the melt, resulting in alloys with a high degree of homogeneity. Typical lithium distributions are presented in Table I. Transverse sections 1/8 in. long were cut from the alloy rods, and each section was split in half longitudinally. One half of each section was analyzed for lithium, and the opposing halves were employed for phase-boundary determinations. Lithium contents were determined by flame photometry with an accuracy of 1 pct of the amount of lithium present. Thermal Treatments. Homogenization and equilibration heat treatments were performed in electrical-resistance furnaces with temperatures controlled to ± 2OC. Calibrated chromel-alumel thermocouples were employed to measure temperature. Homogenization was performed in helium-filled l?yrex tubes for 1 hr at 565°C. The encapsulated specimens were then transferred directly to furnaces maintained at lower temperatures for equilibration. Equilibration times were 2 hr at 550°C, 8 hr at 450°C, 27 hr at 350°c, 90 hr at 250°c, and 285 hr at 150"~. These times were chosen on the basis of conditions employed by previous investigators. Alloys were quenched from the equilibration temperatures by breaking the capsules into a silicone oil bath. By performing all possible operations either in sealed capsules or in a helium-filled drybox, the specimens were given minimum exposure to the atmosphere. Quantitative Metallography. Metallography of Al-Li alloys is difficult because of the atmospheric reactivity of the ß phase. It was found possible, however, to prepare surfaces of good metallographic quality by preventing contact with moisture during preparation. Grinding through 4/0 paper was performed in the drybox. The specimens were then transferred under kerosene to the polishing wheel. Three polishing stages were employed: 25-p alundum with kerosene lubricant on billiard cloth, 1-µ diamond paste on Microcloth, and 1/4-p diamond paste on Microcloth. Between stages the samples were cleaned by rinsing in trichloroethylene and buffing

Jan 1, 1963

By W. J. Loring

It is proposed to describe in this paper as accurately as possible the present practice at the Utica mills, of which I am superintendent. The Utica Company operates three mills, the Madison (40 stamps), the Utica (60 stamps), and the Stickle (60 stamps). My description will be based on the last-named, in which I have experimented more than in either of the other two; but the practice is the same, under the same management, in all three. Everything is run by water-power, under about 420 feet fall at the Utica mill, and 425 feet at the Stickle mill, giving a pressure of about 185 pounds to the square inch. The Madison mill is situated about three-quarters of a mile below the Utica and Stickle mills, and has only some 100 feet fall from one place, and 38 feet fall from the other. The water that runs the Utica and Stickle mills, and all machinery connected with the corresponding mines, is conveyed through ditch and pipe to the Madison mine and mill, where it develops power for the air-compressor and the 40-stamp mill. The mill is run by a

Jan 1, 1899

By J. M. Toguri, H. Flood

The application of the mass action law to the thermodynamic treatment of metal-slag equilibria is discussed. The consideration of the reactions essentially as ionic exchange equilibria is shown to be both an advantage and an aid for the elucidation of the theoretical treatment. This is illustrated by several examples. In general two different methods of application of the mass action law to metal-slag equilibria have been used by different groups of investigators. These could be called the oxide reaction and the ionic reaction approach respectively. At the recent discussion in the metallurgical section of the I.U.P.A.C. Congress in Montreal, 1961,&apos; divergent opinions prevailed regarding the most rational way of applying the mass action law to metal-slag equilibria. This question is of fundamental importance in the treatment and understanding of theoretical chemical metallurgy. Consequently, the following is an attempt to contribute towards its clarification. As an example, the distribution of iron and manganese between molten iron and slag will be considered. I) THE OXIDE EXCHANGE REACTION APPROACH The equilibrium between iron and manganese between molten iron and slag is frequently formulated as an oxide metal exchange reaction as follows:

Jan 1, 1963

By S. G. Cupschalk, F. A. Dahlman, J. J. Wert

Studies have been undertaken to determine the indicidual effects of particle size, degree of long-range ovder, antiphase domain size, and root mean square stran on the microhardness and yield strength of ordered alloys. Dnta have been analyzed for Cu3Pt initzally ordered to a value of 0.82 and after deformations of 1 and 6 pct. It was observed that deformation fleatly reduced the degree of long-range order. Furtherrnore, wztkin this range of relatively small deforntntlons, the average particle size changed very little while the antiphase domain size was greatly reduced. Smultaneosly, the mcrohardness changed by a factor of two durzng the deforrtation process. PREVIOUS studies have reported some of the effects of cold work on the broadening of X-ray diffraction peaks. These investigations were performed on powder and wire samples representing both ordered and disordered states; i.e., the specimens were initially studied in a severly cold-worked condition. By comparing the difference in line shape between the annealed and cold-worked peaks, fundamental information was obtained concerning particle size, strain distribution in different crystallographic directions, degree of long-range order, and change in antiphase domain size. Considerable theoretical work has been done concerning the analysis of diffraction data obtained from cold-worked metals. Stokes&apos; expressed the change in diffraction profiles in terms of Fourier coefficients. Much of the work in this area has been summarized by warren2 in an extensive review article concerning the analysis of plastic deformation by X-ray diffraction. Cohen and Bever3 applied these techniques in studying the effects of cold work on alloy systems exhibiting long-range order. They utilized the Fourier coefficients of fundamental peaks in conjunction with those of the superlattice peaks to determine the change in antiphase domain size. Little work of this nature has been reported for ordered systems that have undergone small degrees of plastic deformation. The purpose of this investiga-tion was to determine the effects of small deformations in such a material with respect to particle size, strain distribution in various crystallographic directions, antiphase domain size, degree of long-range order, and hardness. EXPERIMENTAL PROCEDURE CusPt was used for the initial investigation since the order-disorder transformation takes place with- out a change in crystal structure. The transformation is readily detectable via X-ray diffraction techniques due to the large difference in the scattering factors of copper and platinum. Additionally, the alloy is relatively low melting (approximately 1300°C) and is easily deformable in both the ordered and disordered states. 1) Specimen Preparation and Cold Working. A 100-g, 12-in. diam., cylindrical specimen of Cu3Pt was prepared by melting and casting 99.99 pct pure Cu and Pt i.n vacuo. Prior to any mechanical working, the material was homogenized in a vacuum for 60 hr at 100O0C, and surface defects were removed by machining to a depth of approximately 116 of an in. The material was then cold-rolled, with an intermediate anneal, into a strip approximately 12 in. wide by 14 in. thick. Straightening and flattening removed another 0.025 in. from the thickness. After a recrystallization treatment at 750°C for 30 min, the specimen was slow-cooled from 55OoC, at the rate of 6°C per hr, down to 150°C to induce superlattice formation. This treatment yielded an ASTM grain size of 7 and a degree of long-range order equal to 0.83 0.06. After obtaining X-ray and Knoop hardness data, the sample was cold-rolled approximately 0.75 pct in one pass through a hand-operated jewelers&apos; mill. X-ray and hardness data were again obtained and the specimen was reduced an additional 5.41 pct in a single pass through the mill. 2) X-Ray Measurements. The specimen was examined in the ordered condition and after the two degrees of cold working previously mentioned using a General Electric XRD-5 unit equipped with a spectrometer and scintillation counter. Using Mo-Ka radiation with a zirconium filter, six orders of the 100 reflection were obtained. It was anticipated that point counting would be necessary for an accurate determination of the low-intensity peaks and tails: however, it was demonstrated that, by using a scanning speed of 0.2 deg per min and the appropriate time constant, the recorded data were sufficiently accurate. Thus, for ease of experimental procedure, all peaks were recorded on chart paper. Specimen position in the holder was considered to be insignificant after making a series of measurements of the same peak area in different positions with respect to the beam. Since peak overlapping did occur at high values of 20, it was necessary to separate the peaks graphically prior to analyzing the data in order to minimize this source of error. The peak tails were also carefully drawn to obtain the best possible data. Fourier coefficients of the line profiles were calculated on an IBM 7072 computer, and graphical meth-ods2j3 were employed in analyzing the results. For this type of calculation, in which the line profile is represented by intensities taken at set intervals, the intervals selected must be sufficiently small to give an accurate representation of the line profile. It was decided that for 20 = 0.02 deg the line profiles were

Jan 1, 1967

By Billy L. Crowder, John M. Fairfield

The implantation of B+ , P+, and As&apos; into silicon has been studied with the purpose of making shallow p-n junctions. The influence of such parameters as 1) ion energy, 2) target orientation and temperature, 3) total dose, and 4) annealing schedule was investigated. An energy range of 70 to 300 kev was used for boron and phosphorus implants and up to 500 kev for arsenic. It is found that the experimental projected range agrees well with theory and that shallow junction depths can be made reproducibly. ION implantation has received much attention recently as a technique for doping semiconductors. Specifically, it has the potential of supplementing or replacing the diffusion process as a method for making p-n junctions. In a few specific cases it has been used successfully to make semiconductor junction devices. Potential advantages of ion implantation doping over diffusion techniques are: 1) It affords greater control of shallow junction depths (< 0.2 µ) while maintaining high peak concentrations. This is particularly important for high-speed switching devices, since lower junction capacitances and resistances can be achieved. 2) More precise registration of small planar structures can be realized if proper masking procedures are employed. This advantage is especially useful in the design of high-density integrated circuits. It has been used to advantage in FET fabrication since the edge of the source or drain can be aligned precisely at the edge of the gate electrode.&apos; 3) Ion implanatation permits lower temperatures than diffusion techniques. This factor alleviates the problem of compatibility of diffusivities often encountered when designing multiple-junction structures. Also, the lower temperatures create fewer thermal defects and dislocations, which may account for the high efficiency of some ion-implanted solar cells.2 4) Impurity profiles can be more easily tailored to resemble ideal distributions. Successful exploitation of the potential advantages of ion implantation techniques will depend on increased knowledge and understanding of the subject. The factors likely to be influential in determining impurity distribution profiles in ion-implanted single-crystal targets have been reviewed by J. F. Gibbons.3 In addition to the mass and energy of the implanted ion, the total dose, target orientation, and target temperature are important parameters. The annealing temperature required for removing lattice damage and incorporating the implanted species on an electrically active site is very important. This paper describes an investigation of some of these factors. Implants of boron, phosphorus, and arsenic into silicon have been studied. Energy ranges of 50 to 300 kev were used for boron and phosphorus and up to 500 kev for arsenic. In addition to the implantation energy, the effects of total dose, target temperature, and post implant anneal have been investigated. EXPERIMENTAL PROCEDURE The implantation targets were silicon wafers cut from Czochralski-grown crystals, lapped, and chemically polished. The orientations were (111), (110). and (100) with misorientations of up to 7 deg from the principal axis. For this study, accurate target alignment (i.e., within 0.1 deg) was not available and quoted misorientation values should be regarded as approximate . The implantation equipment consisted of an ion source, a 300-kev linear accelerator tube, an electromagnetic separator, and the associated target supporting and beam focusing assemblies. The ion source was a simple oscillating electron type source,4 which has been described elsewhere.5 The gaseous compounds BF3, PF5, and AsH3 were used as ion sources for B+, P+, As+, and AS+&apos;. Analyzed current levels of up to 20 pamp could be obtained; however, for this investigation target current levels of 1-3 µ amp were usually employed. The analyzed ion beam was collimated through a double slit (1.4 x 0.4 cm) and swept perpendicularly to the long axis of the slit such that an area of about 2 sq cm on each target was covered. Dosages of around 1015 cm-2 were normally employed, but smaller amounts were also used for comparison. A uniform flux density over the bombarded area was assured by the continuous use of profile monitors similar to those described by Wegner and Feigenbaum.6 Post-implant annealing was accomplished in an argon atmosphere in a temperature range of 600" to 950°C. It was not part of the purpose of this investigation to study the annealing kinetics; however, some isochronal and isothermal anneal experiments were conducted to determine the time and temperature necessary to render a reasonably high portion of the implanted ions electrically active (i.e., higher than 50 pct). Post-implant anneal temperatures of around 900° and 600°C were required for boron, and arsenic and phosphorus implants, respectively. Arsenic and phosphorus implants increased in conductivity rather abruptly at the proper anneal temperature of the isochronal curve, but boron increased more gradually over a wider range. Isothermal anneal curves were reasonably flat after 10 min, so an anneal time of 1/2 hr was used for the experimental results described below. The profiling techniques were: 1) neutron activation analysis, 2) differential sheet resistance,7 and 3) junction staining.8 The differential sheet resistance technique is commonly employed in this type of study. Its principal disadvantage is the uncertainty of the ef-

Jan 1, 1970

By Herbert Clark Hoover, Lou Henry Hoover

QUALITIES which the perfect miner should possess and the arguments which are urged for and against the arts of mining and metallurgy, as well as the people occupied in the industry, I have sufficiently discussed in the first Book. Now I have determined to give more ample information concerning the miners. In the first place, it is indispensable that they should worship God with reverence, and that they understand the matters of which I am going to speak, and that they take good care that each individual performs his duties efficiently and diligently. It is decreed by Divine Providence that those who know what they ought to do and then take care to do it properly, for the most part meet with good fortune in all they undertake; on the other hand, misfortune overtakes the indolent and those who are careless in their work. No person indeed can, without peat and sustained effort and labour, store in his mind the knowledge of every portion of the metallic arts which are involved in operating mines. If. a man has the means of paying the necessary expense, he hires as many men as he needs, and sends them to the various works. Thus formerly Sosias, the Thracian, sent into the silver mines a thousand slaves whom he had hired from the Athenian Nicias, the son of Niceratus1. But if a man cannot afford the expenditure he chooses of the various kinds of mining that work which he himself can most easily and efficiently do. Of these kinds, the two most important are the making prospect trenches and the washing of the sands of rivers, for out of these sands are often collected gold dust, or certain black stones from which tin is smelted, or even gems are sometimes found in them ; the trenching occasionally lays bare at the grass-roots veins which are found rich in metals. If therefore by skill or by luck, such sands or veins shall fall into his hands, he will be able to establish his fortune without expenditure, and from poverty rise to wealth. If on the contrary, his hopes are not realised, then he can desist from washing or digging. When anyone, in an endeavour to increase his fortune, meets the expenditure of a mine alone, it is of great importance that he should attend to his works and personally superintend everything that he has ordered to be done. For this reason, he should either have his dwelling at the mine,

Jan 1, 1950

By Gunnar Thaning, Goran Mathisson

The iron ores mined by LKAB in the north of Sweden have excellent beneficiation properties. This gives LKAB a favorable position as regards the production of low silica pellets for direct reduction. LKAB has concentrated on developing and marketing grades of pellets for the Midrex-Purofer-HyL process group, i. e., such direct reduction processes carried out in a shaft furnace or a static bed using reformed natural gas as a reducing agent. The paper deals with properties and quality demands of iron ore pellets for such processes. Matters such as the effect of the residual magnetite in the fired pellets on the degree of metallization, the amount and composition of the slag phase in the pellets, the mechanism of the disintegration during reduction, the state of swelling of the pellets during the conditions prevailing in these processes, the importance of the porosity, the improvement of the reducibility and lowering of the sticking tendency of the pellets by small additions of suitable additives, and the influence of the pellet size are discussed. A special test procedure for direct reduction pellets has been elaborated by LKAB. Thus, three metallurgical properties are routinely determined separately, namely reducibility, reduction strength, and sticking. The test methods are described. Finally the present and future LKAB pellets for direct reduction are presented with respect to chemical analyses and metallurgical properties.

Jan 1, 1980

PUGET SOUND SECTION SIMON H. ASH, Chairman, I. F. LAUCKS, Vice-Chairman, CHARLES SIMENSTAD, Sec.-Treas., 425 Lyon Building, Seattle, Wash. GLENVILLE A. COLLINS, JOHN N. POTT. The Puget Sound Section met at the Arctic Club, Oct. 28, 1916, for the annual meeting. Those present were: Chairman Glenville A. Collins, Vice-Chairman H. L. Manley, Sec.-Treas. Amos Slater, Chester F. Lee, R. P. Tarr, G. E. Rockefeller, Simon Ash, Geo. W. Evans, Joseph Daniels, I. F. Laucks, F. C. Greene, Darsie C. Bard, Marcel Daly, Milnor Roberts, F. A. Hill, Percy E. Wright, and as guest, Mr. Coates of British Columbia. After dinner had been served, Chairman Collins called the meeting to order. The reading of the minutes of the last meeting were suspended upon request of the Secretary. The Secretary read the report from the Committee on the Associated Engineering Societies of Seattle. Upon motion, duly seconded, the report was adopted and placed on file. Mr. Lee, Chairman of the Committee. on the Mining Men&apos;s Convention to be held this coming winter, gave his report orally, and upon motion the committee was continued. The report of the Secretary-Treasurer was read, received, and placed on file.

Jan 3, 1917

By Donald E. Crowell

Due to falling metal prices and depletion of ore reserves, lead- zinc mining in the Leadville, Colo., area gradually came to a halt in the 1950&apos;s. Exploration work continued, however, and by 1969 sufficient ore had been blocked out to warrant sinking a shaft and erecting a new concentrator to treat 700 tpd. The new shaft and concentrator were to be located in Iowa Gulch several miles east of Leadville at an elevation of 11,100 ft. The Leadville project is a joint venture between Newmont Mining Co. and Asarco, with Asarco being the operator. Design work began in the fall of 1969. Engineering was done by Torkelson Engineering Co. of Salt Lake City in conjunction with the central engineering department of Asarco. The plant was constructed by Stearns-Roger Corp. Construction began in the spring of 1970 and the plant went onstream in April 1971.

Jan 11, 1972

By K. G. Davis

Dilute alloys of silver and of thallium in tin have been solidijzed unidirectionally under controlled conditions, to study the segregation associated with a cellular interface under conditions where both thermal and solute convection are present. Autoradiography and radioactive tracer counting techniques were combined with electron-probe microanalysis to study both macro- and microsegregation. It was found that, for concentrations giving only small amounts of constitutional supercooling, cell formation had little effect on the macroscopic distribution of solute along the specimen. At higher concentrations the effective distribution coefficient was higher than that expected for a smooth interface. Node spacing was independent of initial solute content at lower concentrations, becoming greater as keff increased. Silver content at the segregation nodes of silver in tin alloys was independent of initial concentration and considerably in excess of the eutectic composition. SINCE the investigation of cell formation at advancing solid-liquid interfaces by Rutter and Chalmers,&apos; a large volume of work has been dedicated to the determination of solidification conditions under which a planar interface will break down into cellular form. Early experiments were explained satisfactorily by the concept of constitutional supercooling,2 but, due to poor measurement of temperature gradients in the liquid, lack of accurate data on liquid diffusion and equilibrium distribution coefficients, and uncertainty about the effects of thermal and solute convection, these experiments cannot be used as proof for the theory. More recent work, however, has shown that under conditions where convection is eliminated or can be ignored good correlation is observed.3,4 Investigations into segregation at cell caps5 and at cell nodes6-&apos;&apos; have been made, but no measurements appear to have been done on the overall, macroscopic segregation down a unidirectionally solidified rod of material which has solidified with a cellular substructure. This has practical importance in casting, where regions of material with cellular substructure are often encountered, and also in zone refining where the thermal conditions necessary for a planar interface are unattainable. Further, as will be shown, the macroscopic segregation can give information on the following question. Granted that a cellular solid-liquid interface develops from a planar one when the conditions for constitutional supercooling are exceeded, how much supercooling is present after the cells have formed? EXPERIMENTAL PROCEDURE AND RESULTS Specimen Preparation. Specimens 25 cm long with a square cross section 0.6 by 0.6 cm were grown in graphite boats by solidification from one end. Alloy compositions are given in Table I. Two specimens of each composition were grown. The tin was 5-9 grade and the silver and thallium both 4-9 grade. Ag110 and Tl204 were used as tracers. Each composition had the same quantity of tracer so that auto radiographs of specimens containing different concentrations of the same element could be easily compared. Thermocouples inserted through the lid of the boat into a dummy specimen showed that, over the first 10 cm of growth, thermal conditions were quite steady, with a rate of interface advance of 5.8 cm per hr and a temperature gradient in the melt ahead of the interface of 3.0°C per cm. The specimens were seeded from tin crystals of a common orientation to eliminate orientation effects. Dilution of the specimen by seed material was minimized by the provision of a narrow neck between specimen and seed crystal. Macrosegregation. After growth, the specimens were sectioned with a spark cutter. The rods of silver alloy were cut into 1-cm lengths and analyzed for Ag110 using a y -ray counter with fixed geometry. The specimens containing thallium were cut into 2-cm lengths and analyzed for T1 204 by taking 13 counts from each end of the cut lengths through an aperture in lead sheet approximately 0.4 cm square. The results are summarized in Figs. 1 and 2. To find the effective distribution coefficient for the silver in tin alloys under smooth interface conditions, the region of substructure at the bottom surface of one of the 10 ppm specimens, see Fig. 3, was removed by spark machining before counting. Autoradiography. For both alloy systems the samples were polished on sections taken alternately parallel and perpendicular to the growth direction, and autoradiographed by placing the polished surfaces in contact with Kodak "Process Ortho" film. Figs. 3 and 4 show the structures revealed. The alloy containing 10 ppm Ag showed substructure only after a few centimeters of growth, and then substructure was limited to a narrow layer at the base. The "speckled" substructure reported previously in this system4 is here clearly seen to be an intermediate stage between planar and cellular interface conditions. The other samples show a remarkable similarity considering

Jan 1, 1969

By Robert Baschwitz, John Chipman

The distribution of silicon between liquid silver and Fe-Si-C alloys has been studied at 1420oand 1530°C. The data are consistent with earlier studies. New data of Hager on the liquidus lines of the system Ag-Si and the distribution data are used to obtain the activity coefficient of silicon in both liquid phases. Data on the heat of mixing in iron permit accurate extension to 1600°C. Equilibrium data involving SiO2 and silicon in liquid iron together with revised data on the free energy of SiO2 are used to fix the activity of silicon in the infinitely dilute solution. The binary system exhibits strong negative deviation from ideality. At infinite dilution ? Si at 1600" is 1.25 x 10&apos;3, and at concentrations up to NSi = 0.4 the slope d InySi/dNSi has a constant value of r; = 13. It is found that logysi in the ternary solutzon is approximately but not exactly the same function of Nsi + NC as of NSi in the binary. The results are consistent with currently available data on the free energy of Sic and its solubility in molten iron. LIQUID solutions of the system Fe-Si-C have acquired considerable importance as the laboratory prototypes of blast furnace hot metal. Equilibrium studies involving such solutions and slags approximating those of the blast furnace have yielded useful information concerning the thermodynamic properties of blast furnace slags. In studies of this kind great importance attaches to a knowledge of the thermodynamic activity of silicon in the solution as a function of temperature and composition. An attempt was made by Chipman, Fulton, Gokcen, and askey&apos; to evaluate all of the pertinent data on this system and to deduce the desired relation between activity, composition, and temperature. These authors published data on the solubility of graphite and Sic in molten Fe-C-Si solutions and on the distribution of silicon between liquid iron and liquid silver. They showed further how the activity of silicon in very dilute solutions in liquid iron could be calculated from equilibrium data involving the molten alloy and solid SiO,. These calculations rested on the published thermodynamic properties of SiO, in- cluding its heat of formation which at that time was recorded as -209.8 kcal. This value has been under suspicion for some time and has recently been replaced by the concordant results from two independent laboratories2,3 which place the heat of formation of a-quartz at -217.6 kcal. This revision necessitates a re-evaluation not only of the activity of SiO2 in slag but also of silicon in molten iron. It is the purpose of this paper, therefore, to recalculate the activity of silicon, and in furtherance of this objective to present new data on its distribution between liquid Fe-Si-C alloys and liquid silver. HEAT OF SOLUTION OF SILICON IN IRON In order to determine the effect of temperature upon the activity coefficient it is necessary to know the heat of solution of silicon in iron as a function of composition. This is found in the data of Korber and Oelsen4 shown in Fig. 1. The curve corresponds to the following equation, which is of a form suggested by Wagner:5 Here AH is the heat absorbed in kilocalories in forming one gram atom of molten alloy from its molten elements and the N&apos;s are atom fractions. The relative partial molal enthalpies of the components, each referred to its pureliquid state and defined as zFe = aFe - PFe and zsi = HSi — -psi, are shown graphically. At low concentrations zSi = -28.5 kcal, in agreement with Kijrber and Oelsen&apos;s computation. This is in good agreement with the value of -29.3 kcal obtained by Chipman and Grant6 using an entirely different method. ACTIVITY AT INFINITE DILUTION From the known free energy of SiO, it is possible to obtain the activity of silicon in dilute solution in liquid iron from equilibrium studies. The heat of formation of a-quartz is —217.6 kcal and the heat capacity and entropy data are given by Kelley and ~ing.&apos; The free energy of formation of ß-cristo-balite at temperatures above the melting point of silicon is expressed by the following equation: Si(Z) + O2(g) = SiO2 (crist); AF" =-226,500 + 47.50T [I] The value of the deoxidation product for silicon [%Si] x [%O]2 at 1600°C according to Gokcen and chipmans is 2.8 x 10"5, in agreement with results of Hilty and Crafts.9 More recent works of Matoba,

Jan 1, 1963

By H. M. Warrren

IN the past, steam engines were used in practically all cases for driving the machinery, in and about an anthracite breaker, and hence little or no accurate data were available as to the power requirements for starting and operating the individual machines, which make up the complete equipment. It was impossible to segregate the power necessary to drive each individual machine, first, because the equipment was driven in groups, and second, because it was impracticable to obtain graphic, integrated, or instantaneous records of the horsepower used. As a result of these conditions, it was found, when individual electric motors were applied to the various machines, that more accurate and complete data were needed in order to provide motors of the proper power and design for the particular services to be rendered. In order to obtain the desired information, the writers made and collected a number of tests, from time to time, on the individual motor drives in- electrically operated breakers, and as these tests have been of great value, it occurred to them that a paper giving the results might be of service to other engineers interested in similar installations. Table I shows the .results of these tests. All the motors tested were of the three-phase, 60-cycle, 440-volt, induction, squirrel-cage type, except a few, which, on account of size and starting conditions, were of the wound-rotor type. The instruments used in making these tests were: An integrating watt-hour meter, a graphic ammeter, and a graphic voltmeter. These instruments were connected in each motor circuit, and a record of a day&apos;s run of 9 hours was obtained from each machine. From these tests, the running light load, the average all-clay load, and the instantaneous peak readings in amperes, volts, and kilowatt input, were obtained. By means of the characteristic curves obtained from these motors at the factory, the power factor, the efficiency, and the horsepower output were calculated for each particular test. Starting tests were made by the brake-arm method, in which the torque in pounds was measured directly on a spring balance.

Jan 2, 1916

By M. Duclos, A. Sawatzky

A simple model has been developed which describes the steady-state solute distribution in Ti-H type systems above the eutectoid temperature in the presence of a temperature gradient. The solute distribution is dependent on the shape of the phase boundaries. An interesting result, and one that is not observed at steady state in thermal diffusion below the eutectoid temperature, is the existence of a two-phase region. The heat of transport for hydrogen in a titanium, Q*a, over the temperature range 275" to 650.C is determined to be 4500 * 230 cal per mole. The heat of transport for hydrogen in B titanium, QB* over the temperature range 320" to 590.C is found to be 630 ± 200 cal per mole. It is also shown that thermal diffusion provides a method by which phase bounduries above the eutectoid may be determined in Ti-H type systems. IN modern technology materials are being used at constantly increasing temperatures under greater temperature gradients. Thus atomic migration in metal alloys due to a temperature gradient (thermal diffusion) may in some cases occur to an observable extent. The thermal diffusion of hydrogen in zirconium has in recent years received considerable attention1-&apos; because of the use of zirconium alloys in nuclear power reactors. The thermal diffusion kinetics below the eutectoid (547°C) are fairly well understood. At steady state the solid solution, a, and hydride, 6, phases are completely separated with the hydride precipitating at the lower temperatures. No experimental work has been carried out in the a + B region although Droege4 suggested that a complete separation of the two phases, as observed at temperatures below the eutectoid, might not always occur. In the present investigation a simple model has been used to determine the steady-state solute distribution under a temperature gradient in Zr-H type systems heated above the eutectoid temperature. The solute distribution is shown to be dependent on the shape of the phase boundaries in the constitutional diagrams and several typical cases are discussed. The model has been applied to Ti-H. This system was chosen in preference to Zr-H because of its much lower eutectoid temperature (-300°C as compared with 547.C), thereby reducing experimental errors due to oxidation and hydriding. The heats of transport for hydrogen in the a and B phases of titanium also have been determined since they were required to compare the proposed thermal diffusion model with experiment. THEORY In the presence of a temperature gradient the atomic flux in a single-phase region of a two-com-ponent system of which the atoms of only one component are diffusing is given by:&apos; J = - U\dx + RT3 dx) which can be written as: j-D(dn/dt +Q*n/RT2)dt/dx [11 J - -D\dT + RT2)dx [1] where D = diffusion coefficient, n = solute concentration, T = absolute temperature, R = gas constant, dT/dx = temperature gradient, and Q* = heat of transport. At steady state (J = 0) Eq. [I] leads to the solute distribution: n = noexp Q*/RT where no = a constant depending on total solute content. The heat of transport Q* can be experimentally determined from the steady-state distribution. In the present paper we shall determine the solute distribution in systems having the constitutional diagram exemplified by Ti-H shown in Fig. l.&apos; As shown, N,(T) and NB(T) are the equilibrium solute concentrations in the a and 0 phases at temperature T. Lines AA&apos; and CC&apos; define the region of interest to us. The following assumptions are made: 1) Steady-state conditions prevail. 2) In a single-phase region all points on an isotherm have the same thermodynamic potential so that the composition over an isotherm is uniform. If a two-phase region exists, thermodynamic equilibrium is found only at phase interfaces. However, we assume the component of the concentration gradient along an isotherm to be small so that the composition in each phase is approximately the same as at the interface and is given by the constitutional diagram, Fig. 1. 3) There is appreciable diffusion of only one component. 4) We shall consider only the case where Qa*, QB*, and Qg*, the heats of transport for solute diffusion in the a, B, and 6 phases, respectively, are positive. This has been observed for the thermal diffusion of hydrogen in zirconium3 and titanium.10 We will show that the steady-state solute distribution above the eutectoid is primarily determined by the heats of transport and the temperature dependence of Na(T) and Np(T). It may be quite different from the steady-state distribution below the eutectoid. For example, we will see that, under certain conditions,

Jan 1, 1970

By Louis Cates

AT THE annual meeting of the American Institute of Mining and Metallurgical Engineers in February, 1923, the Chairman of the Committee on Ground Movement and Subsidence appointed a subcommittee to work out a form of questionnaire and to collect data on subsidence and ground movement resulting from underground metal- and coal-mining operations, and on ground movement and safe slopes in connection with open-cut metal-mining operations. The author was requested to take charge of the collection of data and the preparation of a questionnaire in connection with the Committee&apos;s studies of open-cut metal-mining operations, this paper is a summary of the work carried on and information received therefrom up to February, 1924. The first approach to the problem of safe slopes is to gather all information that pertains to finished slopes; in other words, the steepest economic angle from the horizontal that will stand in order to uncover the ores to be mined and be safe while the extraction of the ore at the base of these slopes is in progress. Whether or not this angle is 35° or 45° depends on many factors. The number of benches maintained to take care of falling rock and their height and width are direct functions of this overall slope. The slope is here taken to mean the angle from the top edge of the pit through the edges of the respective lower benches to the bottom of the pit. If we accept this definition of the slope, it might save some confusion as there would be a difference if one took the line from the top edge of excavation to the toe of the bottom slope. This latter slope would not be constant, but would vary with the number of benches. The depth of the various ore faces will vary, of course, depending on the deposit; Table 1 shows this to range from 50 ft. to 1100 ft. The geology is an important factor, as are the climatic conditions under which one is operating. A saturated condition in some rock structure causes rock flows; in the Panama Canal excavation, slides have run on a ratio of as low as one on ten, which is a 10 per cent. grade, or a slope of less than 6° with the horizontal. Slopes as steep as 60° have been noted in the Utah Copper operations, so that a wide divergence will possibly be

Jan 8, 1924

By Kenneth L. Cook

THE five serpentine masses exposed within the northern half of Riley County, Fig. 1, constitute a major part of the few exposures of igneous rock in Kansas.&apos; Although not many subsurface data are available for this part of Riley County,2 six deep wellsV indicate that the basement complex lies between 2500 and 3000 ft below the earth&apos;s surface. A northwestward-trending ridge in the present basement surface, which extends across the northern half of Riley County, is indicated on Mettner&apos;s contour map.&apos; The serpentine masses lie in a region that was active during Pennsylvanian and Permian time along two main tectonic trends, which may, in part at least, have developed contemporaneously." One trend is northeasterly, as evidenced by the Nemaha anticline, the Abilene anticline, the Voshell anticline, and many other smaller northeastward-trending folds. The other trend is northwesterly, as evidenced by the central Kansas uplift, the Salina basin syncline, and smaller northwestward-trending folds. The area of the Abilene anticline was actively deformed during much of this time, and the present surface rocks, for the most part Permian in age, show many normal faults." The Bala and Leonardville intrusions lie within a mile of the axis of the Abilene anticline, Fig. 1, as mapped by Wallace Lee;&apos; the Randolph No. 1 and Randolph No. 2 intrusions lie within about 5 miles of the axis; and the Stockdale intrusion lies within about 8 miles of the axis. The igneous rocks have intruded horizontal or gently dipping limestones and shales that are late Permian in age.V he period of intrusion, according to Moore and Landes, was probably Cretaceous.&apos; At present a detailed description of the petrography is available for only the Bala intrusion. Moore and Haynes&apos; describe the rock at Bala as a green, serpentinized, porphyritic, peridotite breccia containing inclusions of shale. The ground mass consists chiefly of serpentine and calcite with considerable chromite (5 to 10 pct) and some magnetite. The phenocrysts consist principally of altered olivine with some altered augite and biotite. Although probably different in petrographic details, all the serpentine masses are somewhat similar in that 1) they consist of a dark green, fine-grained ground mass of igneous rock containing many xeno-liths composed of fragments of the neighboring sedimentary rock; 2) they tend to form small mounds on the landscape, thus indicating their greater resistance to weathering and erosion; and 3) they are magnetic. Previous Magnetic Survey of the Bala Intrusion: To the writer&apos;s knowledge, only the Bala intrusion had been surveyed with a magnetometer prior to the magnetic surveys discussed in this paper. Dreyer8 interprets the intrusion as a vertical, eastward-plunging dike, on the basis of the results of his magnetic survey, Fig. 1, with a vertical magnetom-

Jan 1, 1956

By O. L. Culberson, J. J. McKetta

Experimental and smoothed data are presented for the solubility of methane in water for temperatures of 77, 100, 160. 220. 280, and 340°F at prejsures to 10.000 psia. The minimum solubility phenomenon exists within this temperature range to pressures of 10.000 psia. INTRODUCTION The study of hydrocarhon-water systems has been extended to the determination of the solubility of methane in water at pressures to 10.000 psia. The experimental apparatus, and the technique. are the same as that previously reported.&apos; - In the determination of the solubility of methane in water, only two phases were present at temperatures between 100 and 340°F. these being the vapor phase and the water-rich. liquid phase. The determinations involved the agitation of methane and water in an equilibrium cell. withdrawal of a sample from the liquid phase, and the analysis of the sample. The experimental value; determined in this manner are pre9ented in Table I and in Fig. 1. Since experimental and analytical techniques have improved since the initial experiments with this equipment, it was decided to repeat the 77°F isotherm determinations.&apos; Fig. I shows that the individual results for this isotherm are much

Jan 1, 1951

By J. J. McKetta, O. L. Culberson

Experimental and smoothed data are presented for the solubility of methane in water for temperatures of 77, 100, 160. 220. 280, and 340°F at prejsures to 10.000 psia. The minimum solubility phenomenon exists within this temperature range to pressures of 10.000 psia. INTRODUCTION The study of hydrocarhon-water systems has been extended to the determination of the solubility of methane in water at pressures to 10.000 psia. The experimental apparatus, and the technique. are the same as that previously reported.&apos; - In the determination of the solubility of methane in water, only two phases were present at temperatures between 100 and 340°F. these being the vapor phase and the water-rich. liquid phase. The determinations involved the agitation of methane and water in an equilibrium cell. withdrawal of a sample from the liquid phase, and the analysis of the sample. The experimental value; determined in this manner are pre9ented in Table I and in Fig. 1. Since experimental and analytical techniques have improved since the initial experiments with this equipment, it was decided to repeat the 77°F isotherm determinations.&apos; Fig. I shows that the individual results for this isotherm are much

Jan 1, 1951