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By E. A. Stevens

It has been ascertained in recent years that certain rocktypes, geological formations and structural conditions may be used as fairly reliable guides, when prospecting in recognized mineral belts or milling districts, with a reasonable certainty of discovering "pay-ore;" and that such is considered as a practically established conclusion may be inferred from a perusal of the recent reports of the U. S. Geological Survey and the literature of the several scientific societies discussing mining, geology, and kindred subjects. Cripple Creek is no exception to this conclusion, and the

Jan 1, 1903

By R. G. Ward, A. E. El-Mehairy

A technique was developed to calculate the density of liquid metals from the profile of a weighed levitated drop obtained by emitted light photography and calibration. The density of liquid copper was determined over the temperature range 1370" to 2100°K and expressed with the equation: The molar volumes and thermal coefficients of expansion are calculated. Copper, upon melting, was found to expand 3.34 pct. A knowledge of the density of liquid metals is essential as it is a parameter appearing in most theories of the liquid state. The liquid density is also necessary for the calculation of the commercially important contraction occurring on solidification. Unfortunately good density values are rarely available and the present work was undertaken to establish a new method of density determination free from the limitations of the existing methods. For liquid metals with high melting points, the variation and the limited number of density values reported in the literature have been caused primarily by difficulties in technique, a matter which has been adequately discussed by Urbain.' In all the methods used for measuring the density of the high-melting liquid metals there are sources of error, and corrections have to be made. For example, in the method of balanced columns, the formation of gas bubbles in one or both arms was a great source of error. In the pyknometer3 and immersed-sinker methods, corrections of certain volumes for thermal expansion to the operating temperature exceed 4 pct. In the maximum-bubble method5 a correction for the thermal expansion of the bubble-tube is used (about 1.6 pct); a second correction takes into account the change in the volume of liquid displaced by the bubble-tube (about 3.5 pct). Another method used is based on the shape of a drop of liquid, at rest on an inert refractory plaque, obtained photographically or radiographi-cally. The volume is calculated from the shape, which is sensitive to the surface tension and supporting material, by some intricate empirical relation. The drop contour changes with 90 deg rotation of the support.7 The application of all methods is limited by reaction between liquid metal and the apparatus. The successful stabilization of a mass of liquid metal during levitation melting8 afforded a technique for measuring the density of liquid metals out of contact with solid materials. The technique was developed by using copper as the density of liquid copper has already been studied extensively, thus allowing comparison with the new method. It consists of calculating the volume from the dimensioned profile of the levitated drop obtained by emitted-light photography and careful calibration. The molten egg-shaped drop spins around the magnetic axis of the coil (lined vertically) at a speed which seems to increase with increasing temperature. The method does not involve corrections and the experimental setup allows the use of vacuum or special atmospheres. The maximum operating temperature is limited by excessive evaporation of metal from the droplet. EXPERIMENTAL Levitating System. A stabilizing ring was used in conjunction with a 3-turn levitating coil energized by a 450-kc per sec, 10-kw Toccotron with a high current-low voltage output stabilized to f 1 pet.' APyrex glass tube with a Pyrex Optical flat window inserted through the coil and ring allowed the use of special atmospheres during levitation melting, as shown in Fig. 1. Optical System. Fig. 1 shows the optical arrangement used to photograph the profiles of the drop, parallel and perpendicular to the vertical spinning axis, simultaneously on the same frame of a high-speed 35-mm film. The optical system was adjusted to avoid any distortion of the profiles and to ensure that both profiles are in focus. The length of path from object to objective was about 30 cm, and a magnification factor close to 1 was obtained with the single-lens reflex-camera system. Temperature Measurement and Control. In operation, the specimen temperature was constant to 5 C for a fixed power input to the levitating coil and fixed rate of gas flow through the tube. The temperature was measured by an automatic two-color pyrometer (Coloratio) checked at the melting

Jan 1, 1963

By L. M. Pidgeon, K. T. Aust

There has been considerable interest in the possible use of titanium in magnesium alloys.' Zirconium has shown some promise in this connection2 and its general similarity with titanium suggests that the latter might act in a similar manner. A literature survey revealed that quantitative data on the Mg-Ti system was unavailable. Several patents3 have claimed that titanium additions from 0.2 to 4 pct to magnesium alloys were possible, but no mention was made as to the form in which the titanium existed in the alloy. Kro114 succeeded in introducing only traces of titanium into magnesium by bubbling TiCl4 through the metal under argon or by reacting it with sodium titanium fluoride. The application of theoretical data given by Carapella5 based on Hume-Rothery's principles, involving atomic size factor, crystal structure, valency and the electro-chemical factor, suggests that a Mg-Ti alloy is a favorable case, and the system appeared to warrant experimental examination. Experimental Procedure and Results THERMAL ANALYSIS If titanium is appreciably soluble in magnesium, a change in the melting point of the magnesium might be detectable using standard cooling curve methods. Magnesium was melted in graphite crucibles under an argon atmosphere, the assembly being enclosed in a silica tube. Graphite thermocouple protection tubes served also to stir the melts. The apparatus was very similar to Fig 1, with the addition of a refractory and baffle system to prevent undue heat losses from the top of the crucible. Chromel-alumel thermocouples were calibrated using Al of 99.97 pct purity. Dominion Magnesium Limited sup- plied redistilled high purity magnesium of the analysis given above. Titanium was added in three different forms: 1. Titanium powder —100 mesh, from the Titanium Alloy Manufacturing Co., Niagara Falls, N. Y. 2. Sheet titanium from the U.S. Bureau of Mines, produced by Mg reduction of TiCl4. 3. Magnesium —50 pct titanium master alloy from Metal Hydrides Inc., Beverly, Mass. The melting point of the high purity magnesium used was measured experimentally as 651.0°C. More than a dozen tests were conducted using titanium from the three sources referred to above, in calculated additions up to 20 pct titanium, at temperatures between the melting point and 1000°C and holding periods up to 6 hr. In no case was evidence obtained of solubility of titanium in magnesium, using inverse-rate and time-temperature curves. The melting point of the magnesium was unchanged within the accuracy of measurement, namely -+0.5°C; and no other thermal arrests were detected. Metallographic investigation of the thermal analysis billets indicated that the titanium additions were apparently mechanically entrapped in the magnesium in segregated areas. Consequently, these samples were not analyzed for titanium. The master alloy proved to be a mechanical mixture of titanium particles in a magne- sium matrix. These results indicated that the titanium solubility, if such existed, could not be obtained by the usual thermal methods. X RAY DIFFRACTION INVESTIGATION In an effort to detect solubility of titanium in magnesium, samples were investigated using both the Debye-Scherrer and the Focusing Back-Reflection methods. Filings from samples of the thermal analysis billets and from pure magnesium were annealed in argon one hour at 350°C to relieve mechanical strain. Measurements made of the interplanar spacings showed no difference between the Mg-Ti samples and pure magnesium. The interplanar spacings could be measured to within 0.0002A, and the greatest variation found was 0.0004A, in the back-reflection method. The diffraction lines for magnesium were not shifted by the titanium additions indicating that the solid solubility of titanium in magnesium is of a very low order—less than 0.5 pct. From both diffraction methods, a d or interplanar spacing of 0.817A was obtained for the redistilled high purity magnesium. This latter value is not given in the standard X ray diffraction cards for magnesium metal or vacuum distilled magnesium. Theoretical calculations for a close-packed hexagonal space lattice for magnesium indicate that the planes {2134) should give a line which was found. The relative intensity for this reflection at 0.817A is slightly less than that at 0.870k for magnesium. SOLUBILITY OF TITANIUM IN LIQUID MAGNESIUM The Mg-Mn system was examined by Grogan and Haughton6 who were

Jan 1, 1950

[Trans. No. Place Date Vol. Page 1. Wilkes-Barre, Pa May, '71.. 1 3 2. Bethlehem, I's Aug., '71.. 110 3. Troy, N. Y Nov., '71.. 113 4. Philadelphia, PaFeb., '72.. 117 5. New York, N. YMay, '72120 6. Pittsburgh, Pa Oct., '72.. 125 7. Boston, MassFeb., '73.. 128 8. Philadelphia, Pa.*May, '73.. 23 9. Easton, PaOct., '73.. 27 10. New York, N. Y Feb., '74211] [ ]

Jan 1, 1925

By G. E. Mellor, R. E. Lippoth, T. B. Faddies

The Trixie mine is located in the East Tintic Mining District. Since production began in 1970 over 450 000 tonnes of ore grading 239 grams of silver, 6.9 grams of gold, and 1.2% Cu have been mined from veins in Cambrian Tintic Quartzite. Detailed geologic mapping and extensive sampling are essential for compiling the data base required for efficiently developing and mining known reserves as well as planning exploration and development work. Although the basic techniques used by the geology group at the Trixie were developed many years ago, the reduced activity in underground precious metal mining in the U.S. have made these techniques less familiar to many presently active geologists. The increased activity in precious metals search and exploration again offer cause for the application of these techniques as a prerequisite to efficient exploration, development and production.

Jan 1, 1984

By H. Becke, D. Stolnitz, D. Flatley, W. Kern

Zinc difhsions in gallium arsenide having surface concentrations as low as 5 x 10'' atoms per cu cm have been attained. A multiple-difhsion sequence is employed during which zinc enters the gallium arsenide from a silicon dioxide film in a solid-to-solid diffusion step. The technique is illustrated for the case of a zinc surface concentration of -1 x 1017 atoms per cu cm and a junction depth of 1.2 p. Radiotracer measurements of -0.1-p layers of gallium arsenide are used to delineate the resulting profile. A diffusion coefficient for zinc in pyrolytically deposited silicon dioxide is reported. ZINC is frequently used as an acceptor impurity in gallium arsenide. As examples, p-n junctions are formed using zinc-diffused layers in solar cells, lasers, and varactor diodes. For these purposes surface concentrations of 10'' to over loz0 zinc atoms per cu cm are desired and readily obtained from a vapor source. Diffusion of zinc into gallium arsenide to yield surface concentrations of about 1017 atoms per cu cm, however, is more difficult. For instance, oldstein' reports that large changes in the vapor density of zinc produce only small changes in surface concentration. Such low surface concentrations are necessary in forming the diffused base of a gallium arsenide double-diffused n-p-n transistor in order to obtain an adequate emitter efficiency. An alternative approach to zinc diffusion which can provide reduction in surface concentration of several orders of magnitude is the introduction of the diffusant from a solid source. This can be conveniently accomplished by using oxide films of the type generally employed for selective diffusion masking. Such oxides also serve to prevent the dissociation of the gallium arsenide surface at the high temperatures of diffusion. DIFFUSION PROCEDURE Fig. 1 illustrates the diffusion sequence which is employed for obtaining zinc surface concentrations in the range from 5 x lom to 1 X 10" atoms per cu cm. The description of technique will be given for the instance of -1 x 1017, which is typically utilized in double-diffused gallium arsenide transistor investigations at this laboratory. Tin- or germanium-doped gallium arsenide wafers drawn from crystals grown by horizontal Bridgman or Czochralski techniques are used, with bulk concentrations ranging from 1 to 3 X 10" carrier atoms per cu cm. Each wafer is chemically polished on the (iii) arsenic face using a mixture of five parts concentrated sul-furic acid, one part water, and one part 30 pct hydrogen peroxide at room temperature, followed by rinsing in deionized and quartz-distilled water. Pyrolytic silicon dioxide was chosen as the oxide coating because of the high quality of the films obtainable, the ease of their preparation, and the excellent control over film thickness and uniformity.

Jan 1, 1964

By Harvey S. Mudd

WHEN talking about Europe it is well to endeavor to keep politics and economics apart but they have become so intermingled in recent years that the discussion of one topic inevitably leads to the other. Economic influences formerly prevailed over politics but today national and international economies are governed by political forces. Commerce in raw materials, food, and manufactured products is now so restricted by governmental controls that the capacity of the world to produce and to consume, to exchange goods and to pay for them, cannot be gauged by the past or predicted by a multitude of experts. In prewar days there were some yardsticks but today there are none. Thus it is hazardous to make forecasts, for in all fields of human effort the world has been cast upon an uncharted sea.

Jan 1, 1947

By D. D. Donald

C. J. Barber (U. S. Smelting Refining & Mining Co., Salt Lake City)—In his paper Donald describes how New Jersey Zinc Co. made surveys for a connection between the Ivanhoe and Van Mater shafts at Austin-ville, Va. Except to say that the two faces had to meet "accurately" on line and grade, Donald does not indicate the required precision. Assuming that there were 24 angles in the 11/2-mile traverse and 15 in the one-mile traverse, it can be shown that if the average error in plumbing each shaft was 230" and the average error in measuring each traverse angle was 210". then the average error at the point of -connection would have been about ±1.9 ft normal to the line between the shafts. This calculation assumes that any errors in the triangulation would be negligible compared with the errors in the plumbings and traverses, and it also neglects taping errors. With no constant errors or blunders, the latter would be important only in lines normal to the line between the shafts. To make the average error at the connection less than 1.9 ft would, therefore, require either reducing the error in the plumbings to less than ±30", or that in the traverse angles to less than ±l0", or fewer stations, or a combination of these. Referring briefly to the triangulation, because of the problem of fitting a new triangulation into older surveys of the district the orientation deserved some mention, even though the connection could have been made with an assumed bearing. It would be interesting to know how many triangles were required and what the average summation error was before making any adjustments and without considering the algebraic signs. Perhaps this is referred to indirectly in the statement that the maximum angular error distributed was 2". Turning to the shaft plumbings, it would be helpful to know how many men were employed and how long each shaft was in use. Donald says that the surface positions of W-2 and W-3 were carefully surveyed from the collar position of W-1, without indicating how this was done. The length of the backsight would be particularly important. There must have been some error in setting W-1 vertically below the stations in the headframes. How immovable were the headframes, especially the Van Mater, which appears higher than the Ivanhoe and subject to more vibration because of skip hoisting? Donald does not say whether the plumbing wires had been previously restraightened to minimize spinning (otherwise they behave like weak helical springs). The use of light steel weights is most surprising because there seem to be excellent reasons for using heavier, nonmagnetic weights. Did the shafts contain no steel sets, pipes, power cables, etc., which might attract steel? The plumbing method described by Donald was designed for deep shafts in South Africa but differed from the South African practice in two important respects. As described by Browne,6 in South Africa the line between the wires was made parallel to the long axis of the shaft, whereas in the Ivanhoe shaft the lines between the wires were diagonally across the shaft. The main reason given for the South African practice is to insure that the gravitational attraction between the wires and the rock walls is the same on both wires, and therefore does not affect the bearing of the line between them. It seems probable, however, that the effect of air currents might be minimized in the South African procedure, and might be serious with the wires in the diagonal position at the Ivanhoe shaft. In the South African case cited by Donald the wires were swinging freely (although the plumb bobs were sheltered from air currents) but in the Ivanhoe case they were dampened with the plumb bobs set in water. In the discussion of Browne's paper R. St. J. Rowland said:' It has been the practice for a long time to damp the oscillations by immersing the bobs in oil or water. The time per oscillation is thus increased, thereby extending the time taken to complete the work. The longer the suspended wire the less there is to recommend the practice . . . The theoretical time for one swing of a simple pendulum 1050 ft long is approximately 36 sec, which would be increased by dampening the plumb bob in water. Hence very few complete swings would be observed in the 5 min intervals used at the Ivanhoe shaft. In the two South African cases described by Browne, the length of plumb line in one shaft was 5425 ft, the calculated period of swing was 81.6 sec, the average actual period was 76.6 sec, and 94 complete swings were observed in 2 hr. In the other case the length of plumb line was 3116 ft, the calculated period of swing was 61.8 sec, the average period was 63.5 sec, and 86 complete swings were observed in 1 hr 31 min. Browne concluded that observations of more than 30 swings are not likely to result in sufficient gain in accuracy to be justified. Returning to the Ivanhoe and Van Mater plumbings, an objection to the method used is that all four azimuths were taken from fixed points instead of swinging wires, and that each pair of observations would— barring blunders— check closely, and so perhaps give a false feeling of security. In fact, it seems that only two azimuths were obtained from one plumbing, and not four as stated by Donald. Nevertheless, the tying in of each pair of wires from both sides of the shaft has much to commend it. Donald's description leaves the impression that if each shaft was plumbed only once, the engineers were fortunate indeed if the average error in the underground orientation was as little as 30". Because the survey was done over a period of three years, it seems likely that the plumbings were repeated, perhaps more than once. The underground traverse angles were measured by conventional methods, but because the number of angles in the overlapping traverses was not given, the angular closure given by Donald does not indicate the accuracy with which this was done. Donald's description of a method of taping lines of irregular length is welcome. The literature on taping is usually confined to lines of about one tape length, generally 100 ft. Such lines are rare in metal mining because the time, trouble, and cost of setting points at 100-ft distances underground are not warranted. (Nevertheless civil engineers may go to this expense

Jan 1, 1960

By B. S. Butler

A. D. Mutch (Falconbridge Nickel Mines Ltd., Ona-ping, Ontario)—This contribution is prompted by the fact that the writer has recently published an article'!' which has in part the same general conclusions as B. S. Butler's, namely, the form of the standard mineral paragenesis in hypogene deposits and the parallel transition from early high temperature acid to late low temperature alkaline or neutral solutions. Since the writer also recognizes that he is not fully qualified to discuss the formation of ore deposits as a chemical problem, this discussion will be limited to summarizing other observations and will suggest how Butler's Table II might be made more effective. The form of Butler's table is not unlike that widely used by European geologists'" in which the various minerals are related to the types of ore fluids—peg-matitic, pneumatolic and hydrothermal. Thus the decrease in temperature and change in pH of the ore-bearing fluids as recognized by Butler may also be paralleled by perhaps even greater changes in composition, density, and character. W. H. Newhouse's article:" on the sequence of hypo-gene ore mineral deposition is still one of the most complete analyses of the problem. In it he makes four major observations: 1) The order of O, S, As, Sb is the same as their increasing atomic weights and the same as their melting points. 2) The order of the metallic elements is the same as the Schuermann series. 3) The general mineralogical order is paralleled by decreasing heats of formation. 4) The order is generally in decreasing hardness, higher metal content, and higher specific gravity. The order of 0, S, As, and Bi is also the same as their relative abundance. Another point worth mentioning about this series is that As, Sb, Bi, when abundant, often substitute for sulfur in the early pyrite-like minerals, whereas later in the sequence these elements appear to act more like metals. This behavior may be a further indication of the acid character of the early fluids. C. J. Sullivan"' has attempted to show that the sequence of the metallic elements is related to the order of their melting points and has discussed the interrelationship of the different types of bonding of sulfo-phile and oxiphile elements in minerals. Items 3 and 4 might best be summarized by saying that bonding of the minerals in the series appears to be from ionic to covalent to metallic, the early minerals being light in weight, hard, and near-transparent; the intermediate minerals of intermediate weight, semi-transparent, and semi-conducting; and the end minerals heavy, soft, and malleable, opaque and good conductors. A rapid fall in temperature has been assumed to be the cause of ore deposition in many deposits. Perhaps this in turn is the effect of a rapid release of energy in the form of pressure release and change of volume, the first minerals to form being those with the highest heats of formation which absorb the released energy the most rapidly. Butler's Table II could probably be streamlined and made more effective if the listed compounds were assembled as mineralogical groups as in Dana. Thus the sulfides, arsenides, antimonides, bismuthides, and sulfa salts could be arranged in AX,, AX, A2X2, etc. groups. Since these are continuous substitution series, in which the fields of stability and the heats of formation of the various individual minerals can be fairly regarded as similar, this should be accomplished with no loss of clarity. The occurrence of the individual minerals and the precise sequence of the mineral deposition in any one deposit is probably more dependent on the concentration and relative abundance of the component elements. The assembling of geological data in tabular form such as Butler's Table II will continue to be a very effective method of studying geological phenomena. The importance of this particular problem has been pointed out by C. F. Park,% who concludes that understanding of mechanisms of the standard paragenesis and interrelated problems of mineral zoning in space and time is one of the major keys to classification of ore deposits.

Jan 1, 1959

By J. R. Linney

A HISTORY of the ore-mining and iron-smelting industry of the Adirondacks comprises a century and a half of pioneering by rugged individualists, both men and women. By geographical location, the climate is most severe-long, cold winters with heavy snowfall, and short seasons of vegetation growth; this, together with its remote location from large centers of population, adds considerably to the difficulties of conducting mining operations in this area.

Jan 1, 1943

By Gordon B. Brox, Joseph F. Mcaleer, Charles C. Goddard, Edward P. Shea, Robert G. Ingersoll, Lester G. Zeihen, George J. Burns, John M. Guilbert, Richard N. Miller, Charles Meyer

The Boulder batholith is a composite intrusive in which the Butte quartz monzonite is the dominant rock type. Quartz porphyry dikes intruded the quartz monzonite in directions which were subsequently followed by the eastwest- striking Anaconda system of veins, the earliest major veins in the district. Anaconda veins are faulted by northwest-striking veins of the Blue system, which are most prominent in the central third of the district. Anaconda veins are the major producers in the western third of the district and also in the eastern third, where the "horsetail" zones break off from them. Individual oreshoots are thousands of feet long as well as deep on both systems of veins, but they are generally more persistent and thicker on the Anaconda veins. Viewed broadly, the mineralization in the big veins is arranged in crudely concentric zones of zinc and manganese around a central zone of copper. Only slightly offset from these zones, but earlier structurally, is a zone in which quartz-molybdenite veinlets are prominent. This zone tops at about the 2800 level and widens downward. The pattern of distribution of Cu-Fe-S series minerals in the large veins of the copper zone is not symmetrical with respect to the metal zones. There is a fringe of chalcopyrite-bornite all around the copper front. However, within the copper zone, pyrite-chalcocite-enargitecovellite- digenite assemblages are prevalent near its eastern edge from the 3800 level to the surface, whereas deep on the large Anaconda veins in the western part of the copper zone, chalcopyrite is dominant. Here the chalcopyrite grades upward into bornite-chalcocite ores and eastward into the high-sulfur assemblages of the Leonard mine. Sericite-biotite-K-feldspar alteration envelopes, containing up to about 2 per cent copper as chalcopyrite, are present on some of the quartz-molybdenite veinlets at deep mine levels in the molybdenite zone. These envelopes contrast sharply mineralogically and chemically with the later sericitic and argillic alteration envelopes around Main Stage veins. K'0-Ar'0 ratios indicate that they may be older by about 4 m.y. Secondarily enriched copper ores are mined in the Berkeley pit in the southeastern part of the district. At the present time they account for about half of Butte's production of copper.

Jan 1, 1968

By B. C. Allen

Grain boundary grooving has been studied in chromium, molybdenum, and tungsten under a variety of conditions using high vacuum techniques and tantalum -gettered argon. The average surface free energy of solid chromium, and the chromium-liquid silver interface free energy were respectively found to be 2200 ± 250 and 500 i 130 ergs per sq cm from groove formation kinetics and estimates of pertinent volume difffusion coefficients. The results for chromium were unffected by variations in interstitial content ranging from 0.003 to 0.09 pct C, or 0.003 to 0.03 pct O. Surface diffusion is the primary mechanism of groove formation in chromium under 1 atm argon at 1200" to 140O°C, and is essentially unaffected by 0.003 to 0.09 pct C, 0.003 to 0.03 pct O , metastable nitrogen contents up to -0.01 pct, and up to 2 torr Ag vapor. At higher temperatures, the major mechanism is volume diffusion in argon or evaporation-condensation in stutic vacuum. Surface diffusion occurs in molybdenum at 0.5 to 0.96 and in tungsten at 0.5 to 0.9 of the absolute melting tempera -ture by a single mechanism, possibly by the migration of single adatoms or vacancies. Results were slightly affected by up to 23 tory Sn vapor, and in molybdenum were essentially unaffected by 0.5 Ti or carbon in the range 0.002 to 0.02 pct. Volume difffusion through the liquid is the mechanism of groove formation in chromium-liquid silver at 1200" to 1400°C and in molybdenum-, Mo-0.5Ti-, and tungsten-liquid tin at 1200" to 2000°C. The solid-liquid interface free energies involved were estimated from grooving kanetics. WHEN a grain boundary intersects a solid surface, a groove tends to form along the line of intersection at temperatures above about half the absolute melting point (0.5 TM). The groove progressively grows by preferential atomic migration either by diffusion or evaporation. Establishment of a groove angle occurs in accordance with the grain boundary and surface free energies involved. The motivation for groove formation is a reduction in the total surface free energy of the system. This study is a continuation of previous work on thermal grooving of chromium, molybdenum, and tungsten.&apos; The temperature ranges were extended, and the effect of metallic and interstitial impurities was evaluated. The results were such that certain interface free energies and surface self-diffusion coefficients were deduced from the grooving kinetics. EXPERIMENTAL WORK Materials and Preparation. As indicated in Table I, the 0.05-0.08-cm-thick chromium, molybdenum, and tungsten sheet used was nominally 99.99 pct after recrystallization. Two lots of molybdenum with about the same analysis, Mo-0.5Ti,* and tungsten were ob- *Alloy compsitions are expressed in weight percent . tained commercially. Extruded chromium rod,&apos; prepared from iodide process crystals, was warm rolled to sheet at 700°C. Sheet of three Cr-0 impurity alloys containing up to 0.03 pct 0 was prepared by warm rolling arc melted, extruded, and swaged rod. Two Cr-C impurity alloys containing up to 0.09 pct C were made by equilibrating unalloyed chromium with a known amount of CH4 for 24 hr at 1150°C in previously evacuated quartz capsules. Chromium containing nominally 0.015 and 0.06 pct N was similarly prepared by equilibration with NH3. The sheet was recrystallized to give a stable grain size about equal to the sheet thickness. Molybdenum and Mo-O.5Ti were recrystallized in a tantalum resistance furnace 1 hr at 1 x lo-5 torr at 2300" and 220O°C, respectively. Tungsten was similarly annealed for 1 hr at 2500°C. Chromium and its impurity alloys were outgassed at 1100°C and recrystallized 1 hr at 1700°C under 1 atm Ar. Except for nitrogen, the impurity content stayed roughly constant. Nitrogen in both alloys was reduced to <0.001 pct. In fact, over 80 pct of the added nitrogen was lost after outgassing at llOO°C and annealing sheet 1 hr at 1300°C in argon in the presence of tantalum. Such a rapid loss can be rationalized since -2 torr N are required for equilibrium with 0.04 pct N in solution,3 while the equilibrium pressure is ~10-5 torr over tantalum at 1300°C.4 The recrystallized sheet was cut into small coupons which were metallographically ground and polished on one side with a minimum of grain boundary relief. The surface roughness was on the order of 0.01 µ. The tin and silver used were nominally 99.999 spec-trographically pure. After being outgassed at 1100°C and equilibrated in a molybdenum crucible for 0.5 hr at 1800°C in argon, the tin contained 3 ppm 0, <0.3 ppm N, and 0.1 ppm H. Following outgassing at 900°C and equilibration in a chromium crucible 1 hr at 1400°C in argon, the gas content of the silver was 1 ppm O, <0.5 ppm N, and 0.3 ppm H. Grooving Under Argon or Vacuum. All specimens were placed in unsealed containers made from rod or sheet of the same alloy, thereby enabling the polished surface to achieve gas-solid equilibrium. The annealing fixtures are shown in Fig. 1. The specimen was placed in a resistance furnace with a tantalum or Ta-10W heating element plus tantalum fixtures or radiation shields. Chromium was outgassed at 1100°C, and molybdenum and tungsten were outgassed at 1900°C to 1 x l0-5 torr or at the grooving temperature, whichever was lower. In vacuum anneals, the specimen was then heated directly to the intended grooving temperature. In argon anneals, 99.996 Ar was admitted

Jan 1, 1970

By AIME AIME

BY the end of 1943, the United States will be able to produce aluminum at a rate of 1,150,000 tons a year. How much aluminum is 1,150,000 tons? It is sufficient to replace every railroad passenger car in this country three times a year. Or, it would put a thirty-piece aluminum cooking utensil set in every one of America&apos;s 34,000,000 homes with enough metal left over to make 5,000,000 miles of aluminum transmission cable, such as was used in the electrification of much of rural America. Expansion of aluminum production capacity for the war program has occurred in three steps: (1) expansion by private industry; (2) the letting of contracts by the Defense Plant Corp. for the construction of additional aluminum plants which may remain after the war to compete with existing facilities; and (3) the more recently announced D.P.C. program for the building of emergency plants to make aluminum, using stand-by power available in large metropolitan centers power of relatively higher cost, making it questionable whether such plants, now gravely needed, will be able to compete in a peacetime economy.

Jan 1, 1943

By Robert H. Merrill

During the period from 1960 through 1966, the U.S. Bureau of Mines and Kennecott Copper Corp. performed an experiment to determine the changes in stress, strain, and displacement created by changes in slope angles. The experiment was performed at Kennecott&apos;s Kimbley pit near Ely, Nev. The supporting laboratory studies were made in the Bureau&apos;s Denver Mining Research Center, where final reduction of the data and summary reports are now in progress. The experiment was divided into two phases. The first consisted of the laboratory and field investigations required to select a new slope angle and configuration; the second phase consisted of a full-scale instrumented study in the west wall of the pit. The west slope was changed from an average of 45º to a slope angle that started at 45º on the south wall and gradually in- creased to 57 ½ º at the center of the west wall, and to 61 º on the north wall. The pit was deepened from 500 to about 550 ft, and approximately 2.55 million tons of waste and ore were removed from the wall.

Jan 9, 1969

By R. G. Davies

The activation energy for steady state creep above -500°C is observed to be independent of the applied stress although it varies from -67 kcal per mole at 2 at. pct Si to -100 kcal per mole at 11 at. pct Si due to changes in crystallographic order. The magnitude of the activation energy, by comparison with Fe-A1 alloys, indicates FeSi type of order in certain alloys. X-ray results confirmed the presence of FeSi type of order. It is proposed that dislocation climb is the rate controlling mechanism for all the alloys. It has been demonstrated that when a diffusion mechanism is the rate controlling process, the formation of a superlattice in brass,1 Fe3A1,2 Ni3Fe,3-5 and Feco6 1) increases the creep resistance, and 2) increases the activation energy for steady state creep. Furthermore, a study of creep in Fe-15 to 20 at. pct A1 alloys7 has revealed that as the alloy composition approaches the long-range order field, there is an increase in the activation energy for steady state creep which is thought to be due to an increase in short range order. Fe-A1 and Fe-Si alloys are similar in that they both form the DO3 superlattice in which aluminum or silicon atoms have only iron atoms as first and second nearest neighbors. There are, however, two important differences between the alloy systems: 1) The superlattice formation at -350°C commences at -10 at. pct si8 as compared to -20 at. pct Al,9 and 2) Fe-A1 alloys form a FeAl (B2 type) super-lattice where aluminum atoms have all iron first nearest neighbors even at 22 at. pct Al, but so far no similar FeSi superlattice has been observed. With the similarity between Fe-A1 and Fe-Si alloys in mind, alloys of iron with 2 to 11 at. pct Si were examined for variations with composition of the activation energy for steady state creep and of creep strength. The temperature range of greatest interest was above 1/2 TM (TM is the absolute melting temperature) where it is usually observed that diffusion is the rate controlling process. A subsidiary X-ray investigation of the Fe-Si system was undertaken in an attempt to define the position of the order-disorder boundary as a function of cooling rate. EXPERIMENTAL DETAILS a) Creep. Specimens whose gage length was 1.5 in. and with a cross-section 0.04 by 0.08 in. were strained in tension by a lever-arm arrangement, and the load was adjusted between each creep test to maintain constant stress. The apparatus and mode of operation have been fully described in a previous publication.7 As each test produced a creep strain of 0.25 pct, the variation in stress during the test was negligible. Creep strain was measured at the end of one of the alloy steel grips by a displacement transducer with the out-of-balance potential being recorded on a variable speed recorder. The full-scale deflection of the recorder could be varied in steps to give limits of sensitivity of between 0.1 and 0.001 pct creep strain. The alloys, Table I, were made available by the Metallurgical Department, National Physical Laboratory (N.P.L.), england,10 and by the Research Department, General Electric Co. (G.E.), Schenectady, N.Y. They were hot worked at -850°C, warm worked at 550° to 650°C, and recrystallized in vacuum at -750°C to give a grain diameter of -0.1 mm. All the alloys had a very low impurity content; those from the N.P.L., for which a complete analysis is available,&apos;&apos; show carbon less than 0.026 pct, manganese less than 0.006 pct, and oxygen plus nitrogen less than 0.0024 pct. b) X-ray Procedure. A General Electric XRD-5 X-ray set with a focussing lithium fluoride mono-chromator in the diffracted beam, and a pulse height analyzer to eliminate harmonic wavelengths of the cobalt radiation, was used to investigate the structure of several very fine grained (grain diameter <.01 mm) Fe-Si alloys after the following heat treatments: 1) Quenched from 700°C, 2) slow cooled from 650°C (-40°C per hr), and 3) very slowly cooled from 400° to 100°C (10°C per hr with a 24 hr anneal every 100°C). The method of obtaining the diffraction pattern over the range of 20 from 15 to 45 deg was to count for at least 100 sec every l/3 deg with a slit subtending 1 deg in 20 at the focus; the probable counting error was less than 2 pct.

Jan 1, 1963

By E. J. Efsic, C. M. Wayman

The fcc to bcc y to a transformation in an Fe-24.5 at. pct Pt alloy was studied and found to be martensitic. Large martensite plates are formed in this alloy which are ideal for crystallographic studies; the Ms temperature is about -5°C. Ordering of the parent phase prior to transformation to martensite causes a pronounced lowering of the Ms temperature. For the first time in the case of alloys of iron, measurements of the habit plune, orientation relationship, and magnitude and direction of the shape stvain have been obtained on preselected martensite plates. It is shown that by measuring the initial and displaced (as a result of the shape strain) positions of three or more non-parallel fiducial scratches on one reference surfice the maguitude and direction of the shape strain and the state of distovtion at the parent-mavtensite interface can be determined with a reasonable degree of accuvacy. The agreement between the phenomenolog-cal crystallographic theory of martensitic transformations and the experimental results habit plune, orientation relationship, and nlagnitude and direction of the shape strain) is essentially perfect, and is thought to be the best reported to date for iron alloys. THE comparatively few investigations on binary Fe-Pt alloys have been concerned with magnetic properties, ordered phases, and the equilibrium diagram itself. Various investigations have shown that the equilibrium diagram is of the open y field type; in addition there is a peritectic transformation, a minimum melting point, and three ordered phases: Fe3Pt, FePt, and FePt3. The results of a number of investigators1-6 have shown that the temperature dependence of the y to a (and reverse) transformation in iron-rich alloys is reasonably well-established. The Fe3Pt phase was first noted by Kussman and Rittberg,7 and its existence was later confirmed by Franklin et al,8 Steijn and Donahoe,9 and Berkowitz et al.10 The FePt phase was reported by Isaac and amman&apos; and later confirmed by a host of others.3,6,7,12,13 Kussman and Rittberg7 noted the existence of the superlattice FePt3. Prior to 1956, the 1 to a transformation in iron-rich Fe-Pt alloys was termed "irreversible". In 1957 Klokholm and Donahoe" termed this transformation martensitic, presumably because of its occurrence at temperatures well below those where diffusion normally takes place. This observation served as a point of departure for the present investigation, and in the very early stages of the work to be discussed it was readily verified that the y to a transformation in iron-rich Fe-Pt alloys is indeed martensitic. Quite large martensite plates exhibiting the well-known surface tilt were observed. These plates are ideal in the sense that the boundaries between the parent and product phases were usually very straight. It thus appeared that Fe-Pt martensites would be ideal for crystallographic studies, and this was the purpose of the present investigation. Details of the crystallography of martensitic transformations (particularly for iron alloys) and the phe-nomenological crystallographic theories15-l7 have been discussed many times and thus will require very little elaboration here. The end result of these theories, given in matrix form, is

Jan 1, 1968

By Charles R. Cavanaugh, John F. Elliott

The activity of nickel in liquid Pb-iVi alloys which are rich in lead was measured in the temperature region of 700° to 1100°C by means of the galvanic cell: The electrolyte used was stabilized zirconia. Tlze data were correlated using the a function, and a plot of the temperature coefficient aE/aT All subsequent calculations of the thermodynamic properties are based on these two functions. The activity, activity coefficient, and molar properties of mixing of nickel are reported. Nicke1 shows extreme positive deviations frorn ideality while lead shows a very slight positive deviation in the composition range studied The study of the activity of nickel in liquid Pb-Ni alloys reported herein was undertaken to explore the use of stabilized zirconia, an oxygen-ion electrolyte, with liquid-metal electrodes, and to obtain further information on the thermodynamic properties of the liquid binary Pb-Ni system. The cell The reversible electromotive force of the cell results from the difference in the chemical potential of the oxygen at the two electrodes: po, (left) - p~ (right) = -4E5 [I] The chemical potential of oxygen on the right is fixed by the activity of nickel in the solution and pure solid nickel oxide. That on the left is set by pure solid nickel in equilibrium with pure solid NiO. By definition: Since the chemical potential of nickel is related to the chemical potential of oxygen through the equilibrium constant for the formation of NiO from nickel and oxygen gas, the electromotive force of the cell is also expressed In this case, n is 2, E is the reversible potential of the cell, and 5 is Faraday&apos;s constant. The work of Kuikkola and wagnerl and Schmalz-reid2 has shown that the stabilized zirconia electrolyte is essentially an ionic conductor at the oxygen levels encountered in the experimental arrangement of the work, i .e., PG > 10-l7 atm. THE EXPERIMENTS The advantage of this type of reversible cell over those using a liquid electrolyte is the simplicity arising because the electrolyte also functions as one of the containing crucibles. A further simplification was the choice of the Ni (sat.)-NiO electrode as the standard. This permitted a ready check on the behavior of the electrolyte, as the potential of the cell must become zero when the right electrode becomes saturated with nickel, either because of a change of temperature or because of the addition of nickel to the electrode. It also permitted the potentials being measured to lie in the most satisfactory experimental range of 0 to 100 mv. Although it was not theoretically necessary, lead was included in the standard electrode as it assured good contact between the electrode and electrolyte. Cell Design. The general arrangement of the experimental cell assembly is shown in Fig. l(a) and the details of the cell itself are contained in Fig. l(b). The anode lead wire on the interior of the cell was connected to a coil of perforated sheet nickel. Within this coil were nickel oxide pellets which were held beneath the surface of the liquid Pb-Ni alloy. A disc of nickel oxide was held at the bottom of the external crucible (alumina) by means of the thermocouple protection tube. The nickel oxide disc and pellets were compressed dry at 10,000 psi and sintered at approximately 1000°C for an hour in air. A major experimental difficulty of reversible electromotive force cells with liquid electrodes is the selection of suitable materials for connecting

Jan 1, 1964

[Trans. No.Place Date Vol. Page 1. Wilkes-Barre, Pa.* .... May, &apos;71.. 1 8 2. Bethlehem Pa Aug., &apos;71.. 1 10 3. Troy N. &apos;l Nov., &apos;71.. 1 13 4. Philadelphia, Pa Feb., &apos;72.. 1 &apos;17 5. New York, N. Y.• ....May, &apos;72 1 20 6. Pittsburgh, Pa Oct., &apos;72.. 1 25 7. Boston, Mass Feb., &apos;73.. 1 28 8. Philadelphia, Pa.&apos; May, &apos;73.. 2 3 9. Easton, Pa Oct., &apos;73.. 2 7 10. New York, N. Y Feb.. &apos;74 2 11 11. St. Louis, Mo&apos; May, &apos;74.. 3 3 12. Hazleton, Pa Oct., &apos;74.. 8 8 13. New Haven, Conn....Feb., &apos;75.. 8 15 14. Dover. N. J.&apos; Mav. &apos;75.. 43] [ ]

Jan 1, 1925

By B. Fazan, O. D. Sherby, J. E. Dorn

McLean&apos;s technique was employed to determine the effect of temperature on the contribution of grain boundary shearing to the total creep strain in pure aluminum over the range of 610° to 747°K. The contribution of grain boundary shearing at the same stress was found to depend upon a temperature-compensated time, where the activation energy AH was practically identical with that for total high temperature creep. SEVERAL outstanding investigations by McLeanl-&apos; have demonstrated that the total creep strain in polycrystalline aluminum at 473°K arises from microscopically detectable slip, subgrain tilting, and grain boundary shearing. Whereas microscopically detectable slip arises from dislocations that move out of the grains, subgrain tilting is due to entrapment of dislocations of like sign in subgrain bound-arles. Consequently, creep in polycrystalline aggregates appears to be the resultant of two mechanisms, namely, migration of dislocations and grain boundary shearing. This suggests that an appropriate law for creep should contain two additive terms ?1 = ?d + ?yb where the total creep strain, ?1, depends on the sums of the creep strains arising from motion of dislocations, ?d, and from grain boundary shearing, ?yb. But extensive investigations5 over wide ranges of alloys, grain sizes, temperatures, and stresses have shown that the total creep strain is quite accurately dependent on the single term functional relationship ?1 = f (?), s = constant where s is the stress (constant),* ? = te-?H/RT, t is the time under stress, AH is the activation energy, R is gas constant, and T is absolute temperature. Since Eq. 2 was found to be valid over those ranges where appreciable grain boundary shearing is observed, it appears probable that the activation energy for grain boundary shearing might be identical with the activation energy for migration of dislocations. Thus, under a given stress, it could be thought that where fd and fgb represent the appropriate functions for each mechanism of creep. The primary objective of this investigation was to obtain a direct check on the accuracy of this hypothesis. Experimental Procedure and Results Rolled aluminum sheet (99.987 pct Al), 0.100 in. thick, was used in this investigation. Creep specimens having a 0.25 in. wide, 3 in. long gage section were so machined that their axes were in the rolling direction. All specimens were annealed for 9 hr at 894°K before testing to produce a mean grain diameter of about 0.1 in. One face of each specimen was polished electrolytically in 10 pct HBF4. In order to permit accurate measurements of grain boundary shearing, the polished surface was lightly scribed with a ruling machine accurate to ±0.0001 in. to give a uniform grid of lines which were 0.01 in. apart. Although it was thought that surface working might modify the creep behavior in the vicinity of the scribed grid lines, this technique nonetheless was employed because such local differences in creep properties should not modify seriously the fractions of the total creep strain due to grain boundary shearing or to migration of dislocations. All creep tests were conducted under constant load with an initial stress of 250 psi. The specimen tem-

Jan 1, 1955

[Trans. No,PlaceDate Vol. Page1 1. Wilkes-Barre, Pa*May, &apos;71 13 2, Bethlehem, Pa Aug., &apos;71110 3, Troy, N. Y Nov., &apos;71.. 113 4. Philadelphia, PaFeb,, &apos;72.. 117 5, New York, N, Y.*May, &apos;72,, 120 6. Pittsburgh, Pa Oct,, &apos;72,, 125 7. Boston, Mass Feb,, &apos;73.. 128 8. Philadelphia, Pa,*May, &apos;73., 23 9. Easton, PaOct., &apos;73., 27 10. New York, N, Y Feb., &apos;74,, 211 11. St. Louis, Mo,*May, &apos;74.. 33 12, Hazleton, PaOct., &apos;74., 38 13, New Haven, ConnFeb., &apos;75., 315 14. Dover, N. J,*May, &apos;75.. 43 15, Cleveland, 0Oct,, &apos;75,, 49]

Jan 1, 1928