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By U. F. Kocks

SINGLE slip and a single parallel array of edge dislocations have been obtained in silicon single crystals by homogeneously bending them in a four-point dead-loading device at 1000°C around the [211] axis with [253.] as the tensile axis which encloses an angle of 40° with the glide plane. Other orientations or lower temperatures proved unsuitable. The homogeneity of the bending was checked by the method shown in Fig. 1. The chemically polished specimen was exposed to parallel light from a microscope-stage lamp. The sharpness of the focus of the reflected light is an approximate measure of the circularity of the sample. This method permitted the determination of the actual radius of bent specimens within 10 pct accuracy. The etching solution developed to show up dislocations consisted of the following volume parts: 2 HF, 1 HNO,, 2 CH,COOH, 1 a solution of 5 wt pct of CuNO, in water (Rosi'). The acetic-acid content was adjusted to produce fine well-defined etch-pits in about 2 min at room temperature. The effectiveness of the etch did not depend on the crystal-lographic orientation of the face etched. The number of etch pits produced after a given deformation was checked in the usual way against the Cahn formula' and showed good agreement. As it is to be expected from the orientation of the primary system there are slip steps on the top and bottom faces but not on the side faces (perpendicular to the bending axis), whereas etch pits appear on the side faces but not on the top and bottom faces. This is different only for occasional dislocations of a secondary glide system. All the micrographs included have been taken in places where the most of secondary glide could be seen. From this it is evident that in the homegeneously deformed region the number of secondary dislocations was less than 1 in 1000 of the primary type. Dislocation Distribution—A series of tests with varying amounts of deformation is shown in Figs. 2(a-c). An observation that can readily be made from these pictures is that the linear density of dislocations within slip lines is relatively constant and independent of the amount of deformation. "Slip line" in this context is understood to mean a line that is a straight connection of individual etch pits. The heavily pitted bands which can be seen in each of these three pictures may be resolved fairly definitely, at higher magnifications, into many "slip lines" the distance between them being of the order of 0.5p The distance between dislocations in slip lines is of the order of 2p and it is also fairly constant in going from the neutral zone outward. The higher over-all dislocation density in the outer regions of any sample and the higher total number in a more heavily deformed sample, are effected by a larger number of "slip lines." The relative constancy of the dislocation distance within an individual slip line is surprising. The absence of pile-ups" may imply, if there is no rear- rangement on unloading," that there are no substantial obstacles to slip in this case. It seems that the equilibrium distribution of the dislocations in each active slip plane under the higher external stress on

Jan 1, 1959

By A. R. Krause, C. Laird

In order to establish whether or not there is a real temperature effect in fatigue (independent of environment) , poly crystalline copper and Cu- 7.9 A1 alloy have been cycled at 298° and 7° K in vacuo and the fatigue lives compared with those in air and in liquid nitrogen. The lives of both copper and the alloy were found to be highly temperature-dependent in the absence of environment. This result casts serious doubt on the validity of the cell structure hypothesis for stage I crack propagation as presently formulated, because it predicts that there should be no such tempevnture dependence. On the other hand, the plastic blunling process is consistent with the result. Effects of environment aside, the homogenization of slip which accompanies testing at low temperature, and at low strains, seems to be the main cause for increased fatigue life. At high strain amplitudes, the fatigue lives of wavy slip materials, typically copper, are independent of temperature.' It is well-known, however, that low-strain lives greatly as as the temperature of testing is decreased. By contrast, the lives of planar slip materials, such as Cu-7.9 pct A1 alloy, increase to an even greater extent with decreasing temperature throughout both the high and low strain ranges.1'2'5 The mechanism of this temperature effect is associated with the earliest stages of fatigue failure,'" crack nucleation, and stage I growth,"' which is slow propagation along slip bands to the depth of a few grain diameters. Such life behavior has been interpreted on at least two different bases. On the one hand, those interested in the temperature effect at high strain amplitudes1 believe that stage I growth occurs by the plastic blunting process of crack propagation.7'9 They explain the effect in planar slip materials by the homogenization of slip* which accompanies fatigue testing at low temper- atures and serves both to delay crack nucleation and to decrease the rate of stage I propagation. On the other hand, Holt and Backofen,2 who have studied the effect in low strain fatigue, believe that stage I growth can be interpreted by a cell structure hypothesis.10-12 They have challenged2 the conclusion that there is a real temperature effect in this regime of fatigue testing and have interpreted the increased fatigue lives almost entirely in terms of the "environmental-protective'' effect of the liquid nitrogen and helium baths used to obtain low temperatures. This interpretation by Holt and Backofen2 may offer a means of discriminating between these two mechanisms as currently formulated and used to explain stage I growth. On the basis of the plastic blunting process applied to stage I crack propagation,7* the low strain fatigue lives of both wavy and planar slip materials should be increased with decreasing temperature. This follows because both materials show increased slip homogenization in this strain regime."13 Consequently, crack nucleation in intensified bands will be delayed and the linking of such small cracks into larger stage I cracks will be difficult. In addition, the blunting process required to lengthen a stage I crack from the order of 2 to 10 (where the strain concentration of the crack begins to overcome the slip homogenization property of the material) will also be retarded. These delays will give rise to longer lives in both kinds of material. In contrast to the blunting hypothesis, no temperature dependence has been predicted on the basis of the cell structure hypothesis, because it is well-known that materials cycled at low temperature show no differences in type of dislocation structure for a given strain amplitude.18"20 If the lives of wavy and planar slip materials do show a temperature dependence when the environment is eliminated as a variable, then it is questionable whether cell structures per se have a fundamental role in fatigue fracture. Accordingly, specimens of copper and Cu-7.9 wt pct A1 have been cycled at 298° and 77°K in vacuo and the fatigue lives compared with those in air and in liquid nitrogen, in order to establish whether or not there is a real temperature effect in low strain fatigue. Since it is difficult to measure the strains in specimens when cycled in vacuo, S-N curves have been used as the basis of comparison. In studying the influence of temperature on fatigue life in ordinary environment, Holt and Backofen2 used the superior basis of E-N curves. However, they also published S-N curves and thus established the relationship between E-N and S-N curves. This relationship is used to support the S-N comparison reported in the present investigation. EXPERIMENTAL Materials. The copper employed in this investigation was of 99.99 pct purity and the cu-7.9 pct A1 was prepared from metals of the same purity. The stock, of 3 in. initial diam, was reduced in size by rolling

Jan 1, 1969

[ARTICLE I. NAME AND OBJECT Section 1. This Society shall be known as the Society of Petroleum Engineers of the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. Section 2. The object of the Society of Petroleum Engineers shall be to furnish a medium of cooperation among those interested in the petroleum-natural gas industry an to promote the advancement of this branch of mineral technology through meetings to stimulate the preparation, reading, discussion and circulation of papers connected therewith. ARTICLE II. MEMBERS Section 1. Any person who is a member of AIME may become a member of this Society by the specified process. Section 2. Local organizations may be formed by the Society of Petroleum Engineers as subsidiary units, the membership of which shall be subject to and in accordance with the by-laws of the Institute.]

Jan 1, 1961

By M. J. Sinnott, H. B. Probst

AN extensive survey of the factors which affect austenite grain growth has already been made.' These factors are temperature, time at temperature, rate of heating, initial grain size, hot-working, alloy content, ofheating,initialand rate of cooling from the liquidus-solidus temperature. In the present work, a vacuum-melted temperature.electrolytic iron was used and the variables studies were temperature, time at temperature, and prior ferrite grain size. Other factors were maintained constant. The iron used in this study was vacuum-melted electrolytic iron of nominal composition of impurities of 0.07 wt pct. It was supplied as a ½ in. round cold-drawn bar. This iron was tested in three conditions: as-received, annealed 6 hr at 1200°F, and annealed 6 hr at 1600°F. Samples were ? in. disks cut from the bar. The prior anneals were carried out in vacuum and the isothermal treatments were carried out in vacuum-sealed Vycor tubing. The thermal etch technique was employed to determine the austenite grain size. Prior to sealing the test specimens, one surface of the sample was polished metallographically. This surface, after heating, was examined to determine the austenite grain size, since the austenite boundaries are revealed by thermal etching. This is essentially the only technique available for measuring the austenite grain size of low carbon steels or pure irons without altering the composition. It has been shown to yield results that are in agreement with other methods used for determining austenite grain sizes.' The specimen size was quite large compared to the grain size measured, so inhibition of growth due to size effects is probably negligible. After vacuum sealing, each sample was placed into a furnace at temperature and at the completion of the run was quenched into a mercury bath. The growth temperatures used were 1700°, 1800°, 1900°, and 2000°F controlled to -~10"F. Growth times were varied from 10 to 240 hr. The long times were used in order to eliminate the nucleation and growth effects occurring during the initial transformation. Time was measured from the introduction of the capsule into the hot furnace to the time of quench. Grain-size measurements were made with the use of a grain-size eyepiece of a microscope. By determining the number of grains per square millimeter at X100 and taking the square root of the reciprocal of this number, the average linear dimension of the grains was determined. Figs. 1 and 2 are plots of these data as a function of time and temperature for the various conditions investigated. The variation of D, the linear dimension of the grains, was assumed to follow the equation3 D = A tn. The curves of Fig. 1 were obtained from the data by the use of the least-squares method of analysis. Fig. 1 is for the growth of the as-received stock and Fig. 2 is for growth after prior treatments. Differentiating the foregoing equation gives an expression for the rate of growth dD/dt = G = nAtn-1 = nD/t. Both D and G as functions of t are given in Table I. It should be noted that G is a function of time; the growth rate is rapid at early stages and decreases with increasing time. Since increasing temperature increases the growth rate, it has been common practice to use the empirical relationship G = Go e-Q/RT to relate temperature to growth rate. The growth rate customarily has been taken at constant values of D on the basis that the rate of growth is related to the boundary surface tension and this is measured by the curvature of the boundary. At constant D values, the growth rate is a function of time and temperature. The growth rate can be related however to temperature at constant time, and this has the advantage that under these conditions the growth rate is a function only of temperature. Obviously the Q values, activation energies, obtained for each assumption will not be the same and the question of which is the more correct is a moot one, since the assumed exponential relationship in either case has no particular theoretical significance. By plotting G, at constant grain size, vs 1/T, the activation energy over the temperature range of 1800" to 2000°F is found to vary from 30,000 cal per mol at the smaller grain sizes to 50,000 cal per mol at the larger grain sizes. The 1700°F data do not correlate with the data at higher temperatures. The activation energies for the 1200" and 1600°F prior annealed materials were calculated as 50,000 and 62,000 cal per mol, respectively, using the reciprocal time to a given grain size as a measure of the growth rate. Plotting G, at constant times, vs 1/T yields an activation energy of 12,300 cal per mol for the tem-

Jan 1, 1956

IN the early period of steelmaking, ingot structure and segregation were of no practical importance. Crucible melting required very small ingots that gave little segregation, and a small inserted hot top prevented pipe. As larger ingots were poured from bessemer converters and open-hearth furnaces, segrega- [ ] tion, piping, and gas evolution became increasingly important. The techniques of making semikilled and rimmed ingots were developed with little knowledge of the actual mechanism of the process. The first studies of solidification were made by the Brearleys1 and Gathmann,2- who used stearine to show the effects of shrinkage and mold shape. Fig 11-1 is a picture of a series of stearine ingots at various stages of solidification. These studies showed that the liquid solidifies at a nearly uniform rate from the sides and bottom of the mold and demonstrated the formation of

Jan 1, 1964

By Karl J. Benecke

Though the first patent on a bucket wheel excavator (BWE) was granted in 1881 in the US, this technology was developed in Germany to the high standards of today. However, this development was only possible in parallel with development of shiftable belt conveyors and boom stackers. The combination of these three types of equipment in the open pits of the Federal Republic of Germany has made lignite the cheapest energy source for power generation, despite the low heating value of German lignite on the order of 8500 kJ/kg (3600 Btu/lb) only. Comparing the costs for fuels used in power generating on the basis of their heating value, the relation between lignite, high quality black coal, and imported crude oil is on the order of 1 to 1.5 to 2.5, hence highly in favour of lignite.

Jan 8, 1979

THE late steel strike resulted in an unusual reversal of field when Brazilian interests shipped steel to the United States to assure completion of a blast furnace under construction in Cleveland for the national Volta Redonda mill. The furnace is one of the key factors in an expansion program scheduled to raise Brazilian steel production by 280,000 tons, bringing annual output to 1 million tons. The first consignment shipped to Cleveland included 500 tons of slab and plate steel, and was followed later by another 300 tons. Brazil wants to blow in the furnace by July 1, 1953, and the restricted allocation system brought about by the steel shortage offered a real threat to the deadline. Volta Redonda, established during World War II by Brazilian and American financing, accounts for more than half of Brazil's steel production.

Jan 1, 1952

By E. William Heinrich

With the mounting emphasis on unconventional energy sources, total consumption of lithium minerals will increase significantly in the next decade. The recent development of the lithium battery, for example, may greatly boost the demand for lithium metal. At the same time, the growth in the ceramic, glass, and chemical industries is bound to increase the demand for lithium minerals. In fact, the entire consumption or utilization breakdown of lithium minerals will change considerably from its current pattern. Briefly, today's market for lithium minerals' can be grouped into three categories: (1) Lithium concentrates. Accounting for 57% of market use, these concentrates are beneficiated Li-A1 silicates for ceramic, glass, and glass-ceramic raw materials. The concentrates are chiefly spodumene; inverted iron-depleted beta-spodumene; and petalite or its isochemical decomposition product spodumene + quartz intergrowth ("squi"). In the past, lepidolite has also been used.

Jan 9, 1974

By J. L. O’Brien, M. Suenaga, K. M. Ralls, V. F. Zackay

The effecls of aging a1 400°C on tile resistive transition at 4.2°K of a superconducling 70Zr-30Nb alloy are reporled. Microstrclural changes were studied by critical temperature, resistiue critical field, residual resistiuily, and microhardness measurements and by X-ray diffraction, optical microscoby, ad replication electron microscopy. The result of the aging treat- A defect-free Type 11 superconductor in a magnetic field above Hc1 cannot sustain a transport current runt is a fine array of w-phase pavticles with a mean center to center interparticle spacing of about 800A. At an aging time of 300 hr the maximum onset critical current density is rcached. The particle size at the maximum current density if about 4202. At times longer than 300 hr effective particle impingement leads to lower onset critical current densities. perpendicular to the applied field without power loss in the sample.'-3 This power loss is due to flux line motion caused by the Lorentz force and is manifested by a longitudinal voltage.4-6 When defects are present in the material, flux lines are pinned until the Lorentz force exceeds the "pinning force". That is, it is thought that flux lines reside in free-energy wells existing at the defects, and the critical Lorentz force is that which when integrated over distance will supply the free-energy difference necessary to move the flux

Jan 1, 1968

By E. J. Hall

(Butte Meeting, August, 1913.) THE iron-nail method of assaying has been used for a number of years, but has not met with the approval of all assayers. The method possesses advantages which may be given as follows : (1) no preliminary treatment is required ; (2) a lead button of proper size can be obtained (3) it is economical. On, the other hand, it has its disadvantages, which may be summed up as follows: (1) it is not applicable to ores containing large amounts of impurities other than sulphur, as practically all the base metals will contaminate the lead button ; (2) the slag is unsatisfactory in the larger number of fusions; (3) the method was known to give low silver results under certain conditions and the gold results were questionable. It was with the idea of determining the extent of this latter disadvantage that the following investigation was undertaken. It is well known that the fusion obtained in the lend assay is far more satisfactory than that in the " nails method " for gold and silver. The principal difference in the charges as a class is the presence of considerable reducing agent in the lead charge, and a limited oxidizing action in the nails charge, due to PbO. The possibility of improving the nails fusion by simulating the lead charge was the reason for using argol in some tests, even though there were reasons for expecting this would have -au objectionable effect on the results.

Jan 6, 1913

By W. W. Coblentz

THE constants in question pertain to the total radiation and the spectral radiation of a uniformly heated enclosure, or so-called black body. These constants have been determined for the range within which temperatures can be measured with thermocouples. Conversely, using these constants and suitable instruments, such as an optical pyrometer, for example, it is possible to determine temperatures far above the range attainable with the most refractory thermocouples. The formula of Stefan Boltzmann for expressing the total radiation of a black body is R = kT4 in which k is the coefficient or "constant" under discussion. In view of the fact that total radiation pyrometers are usually calibrated on an arbitrary scale, there is no great demand for an exact value of the coefficient of total radiation in absolute value. However, it is intimately connected with the constant of spectral radiation; hence, an accurate determination of the constant k gives a check on the constant of spectral radiation. The distribution of radiation in the spectrum of a black body is represented by Planck's equation, E? = C1?-5 (e c/?T - 1)-'. The spectral radiation constant c, in this formula, is useful in optical pyrometry and in establishing a high temperature scale. The numerical value of the constant c has been determined in the range of temperatures measurable with thermocouples and, also, by extending the temperature scale to higher temperatures by means of total radiation measurements.

Jan 8, 1919

By K. A. Kiselev, V. I. Zelentsov, V. P. Nebera

INTRODUCTION Most works on flotation of ions and precipitates from solutions have been summarized recently (1-3). Flotation is more desirable than thickening or centrifuging because of higher recovery, productivity, simplicity of apparatus and better economics in general. Electrolytic flotation that utilizes gases is more favorable than other flotation processes because of the following: higher dispersity of gas bubbles, low coalescence of the bubbles, possibility of gradual regulation of the dispersity and other parameters of flotation (4-5). Flotation from solutions is mostly based on the use of alkaline reagents as precipitants (5). Flotation from acid solutions is less common. We used multicomponent solutions with more than 2-3 components, unlike previous research methods. Acidic flotation allows recirculation of solutions to previous operations such as leaching, etc. REAGENTS FOR PRECIPITATION Electroflotation was studied over a wide range of pH with the addition of ferrocyanide, oxyquinoline, hydroxide and carbonate precipitants. In recent works (1,2,6,7) on flotation of Ni, Cu, Zn from alkaline solutions, mostly ferrocyanides were applied. Our choice was oxyquinoline because of the following: 8-oxyquinoline is a nonspecific reagent for many metals, it is readily soluble in acids and alkalis, oxyquinolates of the studied metals are in soluble compounds, the reagent works over a wide range of pH, it is widely available, oxyquinolate precipitates are stable when exposed to air, are readily floatable, and are easily converted to oxides of the metals by sintering.

Jan 1, 1980

By Dorsey A. Lyon, Robert M. Keeney

Page I. Introduction..........234 I1. Chemistry oF Copper Smelting...235 1. Native Copper Ores.......235 2. Oxide and Carbonate Ores....235 3. Sulphide Ores.......236 (a) Elimination of sulphur ...236 III. Reverberatory Copper Smelting...237 IV. Substitution of the Electric Furnace for the Reverberatory Furnace..................... 238 V. Smelting of Fine Michigan Native-copper Concentrates in the Electric Furnace.................. 239 1. Conclusions.................240 VI. Proposed Process for Electric melting of Fine Native-copper Concentrates.................. 241 VII. OrdINary Copper Blast Furnace 'Smelting......... 245 1. Prerequisites.................. 245 2. Losses .................... 247 VIII. Experimental Data on the Electric Smelting of Raw Sulphide. Oxidized and Carbonate Ores............. 248 1. Vattier's experiment................ 248 2. Wolkoff's experiments................ 249 3. Experiments of Stephan.............. 250 (a) Conclusions of Stephan ............ 251 IX. Smelting of Sulphide Ores in the Electric Furnace...... 251 1. Ores Treated.................. 252 2. Conclusions................... 253 X. ELectric Furnace vs. the Reverberatory Furnace and Blast Furnace as a Melting Agent.............. 253 XI. Smelting of Sulphide Ores without Roasting or Partial Pyritic Smelting............254 XII. The Electric Blast Furnace vs. the Copper Blast Furnace for Partial Pyritic Smelting.......259 1. Metallurgical conditions......259 2. Mechanical considerations......259 3. Comparison of costs.......260 (a) General considerations .....260 (b) Cost of plant........260 (c) Amount of electrical energy...260 (d) Cost of smelting.......261 (e) Cost of electrodes........262 XIII. The Use of the Electric Furnace in the Smelting of PyRITIc ORES : 262 XIV. Summary...................... 264

Jan 1, 1914

By W. B. Dancy, A. Adams

Laboratory test work on heavy liquid separation of sylvite from halite is reported. Numerous tests were run on sylvite ore sized in the ranges of 4x20 mesh, 10x65 mesh, 8x100 mesh, -8 mesh and -10 mesh with heavy liquids in the range of 2.05 to 2.15 sp gr. From the test results, it was concluded that, with the type of ore under study and a size in the range of -8 mesh, a recovery as high as 90% could be achieved with a product grade of 70% KCl. However, a final product at an acceptable recovery cannot be made with one pass, and the float must either be further processed with heavy liquids or dried and sent to a conventional froth flotation circuit. Potash ores occurring in this country consist essentially of sylvite and halite plus minor amounts of magnesium sulfate salts and montmoril-lonite-type clays. Recovery of potash minerals from evaporite ores in the North American potash fields is accomplished almost exclusively by use of amine flotation. European practice involves froth flotation as well as solution-crystallization processes. Laboratory and pilot plant test work has been reported in Europe and the U. S. on the application of heavy media separation to potash ore beneficiation. Work was probably discontinued because of lack of ore with the required very coarse liberation characteristics (1/8 to 1/2 in. liberation size). Sylvite, with a gravity of 1.99, and halite, with a gravity of 2.17, appear to be ideal for separation by heavy liquids, which are now available in gravities from 1.59 to 2.95. This paper reviews preliminary results obtained from laboratory test work on heavy liquid separation of sylvite from halite. TEST WORK The heavy liquids used in the tests under discussion were chlorobromethane, with a specific gravity of 1.923, and dibromethane, with a gravity of 2.490. These liquids, completely miscible, were combined in the proportions needed to give a mixture having the desired specific gravity. Feed for the laboratory tests was mine-run ore screened to the desired mesh sizes. In conducting the tests, the sample was fed at a constant rate into a stream of heavy liquid and the mixture directed into a small separatory vessel. The float overflowed into a collecting pan while the sink collected in the bottom of the separatory vessel and was removed at the end of the test. Approximately 500 g of feed constituted a charge. Pulp density of the feed was kept low to prevent particle to particle interference in separation. With feed in the range of 8x100 mesh, a pulp density of under 10% solids by weight was found advisable. With coarser feed the pulp density could be carried as high as 15% solids. Time of separation was very rapid. In the case of 4x20-mesh material, separation was effected in 15 to 30 sec; with -10-mesh feed, separation required about 1 to 2 min. SPECIAL EQUIPMENT Since heavy liquids are toxic to varying degrees, all separatory work was carried out in a standard laboratory fume hood. It was noted that complete removal of fumes was not being effected; therefore the hood construction was modified, resulting in a completely satisfactory arrangement for heavy liquid test work. In the interest of safety, details of this fume hood are reported here. Unlike most fumes, heavy liquid fumes tend to settle and flow like water, rather than to rise like a gas. Working on this assumption, a standard water drain was installed in the hood. Across the front of the hood a 1-in. barrier was constructed. In the rear of the hood a false back was installed, with an adjustable sliding door on both the bottom and top of this panel. As shown in Fig. 1, the exhaust fan pulled a vacuum behind the barrier, sucking the heavy fumes from the bottom of the hood. Another addition was the drying box, shown to the right of the hood. This is simply a box covered on top with hardware cloth and connected by a 6-in. inlet to the hood. Sample trays made of fine mesh wire filter screens were found ideal for drying samples. With this arrangement, air flowed completely through the sample and all fumes were drawn into the hood. In use, it was found effective to cover with a

Jan 1, 1963

By J. Hudy

An investigation has been made to determine the applicability of the Cendrex X-ray instrument for the measurement of the ash contents of washed bituminous coal products. The results obtained for selected products from five preparation plants in the northern Appalachian region are described. Emphasis of the study was placed on low-ash bituminous coals suit-able for utility or metallurgical markets. There was good agreement between the results obtained by conventional ash determination methods and by the Cendrex for all the products tested. A principal disadvantage of coal in competition with other fuels has been its inconsistent quality, especially with respect to ash content. Mine rnechanization and production from coalbeds of inferior quality have accentuated this failing. Present quality control methods in coal preparation plants are inadequate because (1) control samples taken over a production shift only serve to give the average quality of the product, (2) conventional sampling and analysis data are usually not available at the time a shipment is scheduled, and (3) the plant operator does not have the use of such data when the coal is being processed so that operating conditions may be adjusted for correcting variations in quality. Thus, the development and use of continuous-control monitoring instruments is of prime importance. The Federal Bureau of Mines arranged to investigate an instrument using x-rays for rapid continuous ash determinations. Developed by the Dutch State Mines and first described in 1958,' this instrument, which has found widespread acceptance in Europe, is designed to provide ash analysis of any desired coal feed or product stream with only a five-minute time lag between sample collection and analytical results. With limit controls, this unit could be used to feed back signals to preset the separating gravity of coal washers, control the ratio of various coals needed to produce an acceptable blend, and permit the sorting of a washed product into two qualities, one which is below and the other which is above a prescribed ash content. This unit can also be used discontinuously for rapid determination of coal samples taken in the usual manner. THEORY Di jkstra and Sieswerda of the Dutch State Mines studied the effect of chemical composition and ash content on the absorption coefficient of coal with the transmitted radiation method.' They found that with an X-ray wavelength of 1.79 A and values calculated for the absorption coefficients of ash and combustibles, the absorption coefficient of coal gave a linear relationship when plotted against the ash content. Thus, a method of measuring the absorption coefficient of coal could also be used to measure the ash content. However, practical attempts to measure the ash content of coal by comparing the intensities of the transmitted X-rays failed. The absorption coefficient of coal can also be obtained by irradiating a layer of coal with x-rays and measuring the intensity of the diffused reflection (backscatter method). The relationship between the diffused reflection and the ash content is actually hyperbolic but approximates a straight line over a narrow range. A measuring circuit that balanced the difference in intensity of the reflected radiation from a standard surface against that from a coal sample was used. By plotting this difference of reflected radiation against the ash content, a curve which approximated a straight line over a range of 8 percentage points of ash was obtained. DESCRIPTION OF EQUIPMENT The apparatus performs two distinct functions: (1) the preparation of the sample to a suitable size consist and moisture content for delivery to the x-ray element, and (2) the measurement of the ash content by the x-ray element. In a continuous operation the coal sample is delivered to a conditioner where it is dried to a maximum of 1% surface moisture and pulverized in a high speed mill to -48-mesh. This material is fed, at a rate of 250-300 gpm onto a rotating disk, shown in Fig. 1, where it is mixed with material already present. The mixture is rotated on the disk and

Jan 1, 1969

By V. A. Phillips

Transmission-electron micrographs of electro-thinned samples of bulk-aged Cu-3.1 pet Co alloy show an aging sequence, supersaturated solid solution — coherent particles — quasi -coherent particles — noncoherent particles. Hardening is due to precipitation of coherent spherical fee coball-rich particles showing coherency strain fields, which are resolved at between 15 and 30A diameter. Loss of- full coherency did not occur until well into the overaged region, even with the assistance of deformation after aging. Different average particle diameters of 123, 92, and 149 ± 10Å were observed in samples aged to peak yield strength at 600°, 650°, and 700°C, respectively, indicating that there is no critical size for peak hardening. Noncoherent particles tended to develop (111) faces and became octahedral in shape. Dislocations tended to nucleate spherical coherent particles which eventually grew together forming large elongated particles. The surface energy of a noncoherent (low-angle) inter-phase boundary is estimated to he about 50 ergs per sq cm. A number of particle lining-up phenomena were observed. Overaging is principally attributed to increase in particle spacing, progressive loss of coherency, and increase in amount of discontinzdous precipitation. COPPER dissolves about 5.6 at. pet (5.2 wt pet) of cobalt at 1110oC1 and the solubility decreases to 0.75 at. petl (0.54 at. pet)2 at 650°C and to 0.1 at. pet or less at lower temperature.' It has been known for many years3-5 that Cu-Co alloys are capable of age hardening. Since cobalt is fee above 417°C and its atom size is only about 2 pet smaller than that of copper, precipitation of coherent particles would be expected. The equilibrium phase precipitated at 700°C and below contains about 10 pet Cu in solution which tends to stabilize the fee structure, lowering the transformation temperature to 340oc.l The alloy is known to undergo discontinuous precipitation in addition to general precipitation; while the former can be seen with an optical microscope, the latter precipitates are not visible except in the grosly overaged condition.5, 6 Extensive use has therefore been made of the ferromagnetic properties of the precipitate in order to follow the course of aging, and it has proved possible to measure the average particle size, spacing, approximate shape, and volume fraction and to determine that the particles are coherent without ever seeing a particle (see for example Refs. 2, 7, and 8). The magnetic measurements of particle size are limited to diameters below about 120Å.7 The present study was undertaken using the techniques of transmission-electron microscopy in order to check the above conclusions, to extend the previous magnetic work to larger particle sizes, and to attempt a more detailed correlation of properties and structure. A portion of this work has already been published.9-11 The present paper is concerned with the metallographic features of precipitation in relation to aging curves. Bonar and Kelly12'13 have published preliminary results of a similar study on single crystals of Cu-2 at. pet Co. EXPERIMENTAL Preparation of Alloy. A Cu-Co alloy, containing 3.12 wt pet (3.36 at. pet) Co by analysis, was prepared from 99.999 pet purity oxygen-free copper and electrolytic-grade cobalt. The alloy was melted and cast in vacuo in a high-frequency furnace using a graphite crucible and mold: Analysis showed chat 0.004 pet C was picked up during melting. The 1-1/2-lb ingot was homogenized in hydrogen for 24 hr at 1000°C. Slices were cold-rolled to 0.005 or 0.003 in. thickness, with an intermediate 650°C anneal in hydrogen at 0.080 in. thickness. Batches of six to ten strips were solution-treated in sealed-off quartz tubes in high vacuum in a vertical furnace and quenched by dropping into iced brine containing a device which snapped off the nose of the tube. Solution treatment consisted of 1 hr at 990°C or 2 hr at 965°C. The latter was employed for all mechanical-property studies, since a tendency was noted for the higher temperature to give porous material. Strips were usually aged individually in a horizontal vacuum furnace, inserting into the hot zone and withdrawing into a cold zone without breaking the vacuum. This method gave a rapid heating rate, permitting the use of short aging times. In some cases, particularly for the longer aging times at the higher temperatures, samples were sealed individually in quartz tubes in high

Jan 1, 1964

By O. N. Carlson, W. M. Paulson

A phase diagram is proposed for the Y-C system based on the vesults of thermal analyses, microscopic obsevvations, and X-ray diffraction studies. Three intermediate phases occur in the system: a congru-ently melting fcc phase with a wide range of homogeneity about the composition Y2C, an intermediate solid-solution region between 55 and 58 at. pct C, and a bct dicarbide melting congruently at 2415°C. All three compounds undergo a phase transformation at elezlated temperatures. A continuous serzes of solzd solutions exists between the fcc phase and the high-temperature form of YC2 with a maximum in the solidus at 2000°C and 30 at. pct C and a minimum at 1805°C and 54 at. pct C. THIS investigation of the Y-C system was undertaken as part of a nuclear materials development program. Yttrium-base alloys are of interest as possible containers for liquid metals, and carbides are currently receiving increased attention as high-temperature materials for advanced reactors and other applications. Previous work on this system was limited in scope, and the results were somewhat inconclusive and at times contradictory. Spedding et al.&apos; reported the existence of a triyttrium carbide having an fcc structure with a wide range of homogeneity and Dean et a1.2 reported the existence of a rhombohedra1 phase having the stoichiometry of Y2C. Bachella et a1.3 observed that the latter was the result of ordering of carbon atoms in the fcc solid solution. The ordering range was placed at 800" to 1000°C. Vickery et a1.4 reported a high-melting compound which they identified as yttrium dicarbide, and Spedding and coworkers1 determined the structure of this phase as bct with lattice parameters a = 3.66 and c = 6.17A. Samsonov et al.5 reported the melting point of YC2 as 2300" * 50°C. Recently Bowman et a1.6 found a transformation in the dicarbide from the tetragonal to an fcc form at 1320 20°C. Samsonov and coworkers7 reported a monocarbide of yttrium melting at 1950" * 20°C and also a sesqui-carbide melting at 1800" * 50°C. The existence of the latter has also been indicated by others,1&apos;8 but neither compound has been definitely established. The Y-C phase diagram shown in Fig. 1 was proposed by Chubb and Keller8 in 1964 based on the data available at that time. The tentative nature of this diagram together with the uncertain status of the compounds indicated that additional work on this system was needed. EXPERIMENTAL PROCEDURE Yttrium metal of 99.9 pct purity was prepared for use in this study by the reduction of YCl, with calcium to form a sponge product.9 The major impurities in this material were as follows: 100 ppm C, 150 pprn H, 20 ppm N, 300 to 1000 ppm O, <20 ppm Ca, <100 ppm Cr, <80 ppm Cu, 150 ppm Fe, <30 pprn Mg, <400 ppm Ta, and <100 ppm Ti. Alloys were prepared by arc melting yttrium sponge together with pieces of high-purity graphite rod in a purified argon atmosphere. Homogeneity was insured by repeated melting, inverting the ingot between melts.

Jan 1, 1969

By H. W. Reinhardt, J. W. Dally

A dynamic photoelastic analysis of stress waves interacting with a free surface is described. The free surface is that of a bench with a fixed bottom so common in quarry applications. The stress waves are generated by line charges of lead azide (Pb N,). Four models of identical geometry are investigated with the direction of detonation of the line charge varied between the four models. Dynamic photoelastic patterns are recorded and analyzed to indicate which method of detonating the line charge produced the largest magnitude of tension at the free surface. The mechanics of rock breakage by means of explosives has received considerable treatment by many investigators including Duvall, Obert, Broberg, Rinehart, and Langefors1-11 over the past two decades. Indeed in more recent years several texts12-15 have been written on the topic, treating a wide variety of subjects which are logically related to the modern technique of rock blasting. In rock blasting the chemical energy of a concentrated explosive contained in a relatively small diameter borehole is utilized to fragment the rock. The explosive is transformed into a gas with enormous pressures which exceed 10-5 bars18 This high pressure shatters the rock in the area adjacent to the borehole and produces dilatational and distortional stress waves which propagate radially away from the borehole. The state of stress associated with these outgoing waves produces a system of cracks which extend for a few feet from the borehole. The breakage produced in this manner is limited as the dynamic stress in the pulse attenuates markedly with distance. In the absence of a free surface, the stress wave propagates away from the source without further fracture. With a free face of rock near the drill hole, another mode of breakage occurs which is due to scabbing failure of the layer of rock adjacent to the free face. These scabbing failures are produced by the reflection of the incident waves and the conversion of compressive stresses into tensile stresses sufficiently large to fracture the rock. The detailed nature of the interaction of the stress waves with the free surface is complex and difficult to treat analytically. However, dynamic photoelasticity offers an experimental approach which gives a fullfield visual display of propagating stress waves and the reflection process. Applications of static photoelasticity to solution of problems related to mining technology have become relatively common (see, for instance, Refs. 17 and 18) with a plastic model loaded to produce a state of stress representative of that occurring in the workings of a mine. The application of dynamic photoelasticity is ex tremely limited. Tandanand and Hartman19 have used a multiple spark camera to study fracture in glass and plastic plates impacted by a chisel-shaped tool. This paper describes a dynamic photoelastic analysis of stress waves interacting with a free surface. The free surface is that of a bench with a fixed bottom so common in quarry applications. The stress waves are generated by line charges of lead azide (Pb-N6). Four models of identical geometry are investigated with the direction of detonation of the line charge varied between the four models. Dynamic photoelastic patterns are recorded and analyzed to indicate which method of detonating the line charge produced the largest magnitude of tension at the free surface. Experimental Procedure The model illustrated in [Fig. 1] was fabricated from a sheet of Columbia Resin CR-39 to represent a bench with a fixed bottom. Properties of the CR-39 pertaining to these dynamic experiments are listed in [Table 1]. Scribe lines on 1-in. centers are used to identify locations along the bench face. The bench height was 8 in., the burden was 3 in., and the overall dimensions of the sheet, 16 and 18 in., were large enough to eliminate reflections from nonessential boundaries during the period of observation of the dynamic event. To simulate a charge in a borehole, a groove 0.062 in. wide and 0.080 in. deep groove was cut into the sheet from one side. The lower end of the groove was 1 in. or 1/3 the burden distance below the bottom of the bench. The upper end of the groove was 3 in. or one times the burden distance below the upper level of the bench. The groove was packed with 60 mg of Pb No per in. of length, and ignited with a bridge wire detonator. Four different ignition procedures were used to examine the effects of detonation direction on the stress wave interaction with the free face of the bench. In Test 1 the line charge was ignited at the top and the line charge detonated downward. In Test 2 the line charge was ignited at the bottom and the charge burned upward. In Test 3 the charge was ignited in the center with the top half burning upward and the bottom half burning downward. Finally in Test 4 the line charge was ignited at both ends simultaneously. Sixteen high-speed photographs of the photoelastic fringe patterns representing the stress wave propagation were recorded for each of the tests. A Cranz-Schardin multiple spark gap camera 20,21 was operated at framing rates which were systematically varied from 110,000 to 250,000 frames per sec during each test.

Jan 1, 1972

By A. J. Griest, P. D. Frost, J. R. Doig

During the past 5 years, research directed toward the development of titanium alloys having improved strength-ductility relationships and heat treatability has been carried out at Battelle for the U. S. Air Force.1"3 In the course of this work, a method of heat treating ß-stabilized titanium alloys was developed which produced a wide range of useful properties.4 The heat treatment consisted of two steps: a) solution treating at temperatures in the a-ß phase region, and b) overaging at a lower temperature in the range 800°to 1100°F. Corollary to the alloy development work, research was conducted on the mechanism of the heat-treatment reaction. The investigations of Frost and co-workers on isothermal transformation in Ti-Cr5 and Ti-Mn8 alloys disclosed the existence of the transition phase, w, during the course of the decomposition of metastable ß phase. Subsequent work at Battelle7,8 &apos;and at Case Institute by Brotzen and co-workerss further clarified the nature of the decomposition process. Beta decomposition was found to proceed by the following series of reactions: 1 2 3 4 a + Ti, My (in eutectoid systems). ßo, ßr, and ßU refer to ß phase of original, enriched, and ultimate alloy contents, respectively. Omega is a transition phase having a complex structure. 10-13 Step 4, of course, occurs only in ß-eutectoid systems. This paper presents data correlating transformation behavior with mechanical properties for the following alloys: Ti-8Mn, Ti-8Mn-2A1, Ti-4Mn-4A1, Ti-6Al-4V, and Ti-4Fe. The isothermal decomposition of ß in titanium-manganese alloys of similar composition has been investigated by Frost and coworkers8 and the effect of various annealing treatments on alloys in this system has been studied by Holden, Ogden, and Jaffee.14 The compositions Ti-8Mn-2Al, Ti-4Mn-4A1, and Ti-6A1-4V, were studied in the present work in an effort to define more clearly the effect of aluminum on the response to solution and aging treatments. Ogden, Holden, and Jaffee15 have invesitgated the effect of aluminum on the response of a similar alloy (Ti-8.8Mn-2.46A1) to annealing treatments, and Luini and Lee16 have made an exploratory investigation of the heat-treatability of the Ti-4Mn-4Al alloy. The Ti-4Fe alloy was studied as an example of a moderate1y active eutectoid system. Holden, Ogden, and Jaffee 17 have studied Ti-Fe alloys and have presented some hardness data for aging at 400°C for alloys of Ti-2.56, 5.01, and 7.35 iron after quenching from the a-ß field (750°C). EXPERIMENTAL PROCEDURES The experimental procedures generally used in the precipitation-hardening study are outlined in the following sections. Departures from these techniques are noted in the discussions of the individual alloys. Table I presents the nominal and actual compositions of the alloys studied, together with the swaging and rolling temperatures. In all cases, these temperatures were in the a-ß field and the microstructures consisted of an equiaxed a-ß mixture. Melting and Fabrication—Except for the commer-

Jan 1, 1960

By W. V. Green

The creep-rupture behavior of commercial powder-metallurgy tungsten rod is reported for temperatures of 2250°, 2500°, 2700°, and 2800°C, stresses up to 7000 psi, and times up to 4 hr. The temperature dependence and the stress dependence of creep rates are evaluated. Rupture time is fitted to the Larson-Miller parameter and compared to lower-temperature and higher stress results reported by pugh.4 THE tensile strength of single-crystal wire1 and of polycrystalline wire2 have been measured by Goucher. More recently Bechtold3 and pugh4 have studied the mechanical properties of tungsten rod between room temperature and 1200°C. Since tungsten has the highest melting point of all metals, it should retain useful strength to very high temperatures, and should find many applications in missiles, rockets, and so forth. Therefore, the mechanical usefulness of polycrystalline tungsten rod was investigated in the 2250" to 2800°C temperature range by short-time creep-rupture tests. MATERIALS TESTED Creep specimens were machined from 1/2-in. round commercial tungsten rod which was manufactured from powder by cold pressing, sintering, and hot swaging. Purity reported by the vendor was 99.95 pct W. Spectrochemical analyses showed "traces" (less than 0.01 pct) of silicon, iron, and titanium, and "faint traces" (less than 0.001 pct) of calcium and manganese. Carbon content was 30 ppm and nitrogen content was 70 to 110 ppm. No oxygen analysis was obtained. Room-temperature stress-strain tests on the as-received tungsten gave badly scattered results. Threaded end specimens broke at the threads. When these specimens were retested using shoulder grips, the specimens broke at the shoulders. No fractures occurred in the gage lengths. The fracture stresses were: 127,000; 137,000; and 154,000 psi for three specimens which fractured at the shoulders. The microstructure of the as-received tungsten rod is shown in Fig. 1. SPECIMENS USED Fig. 2 shows the two types of creep specimens tested. The threaded-end type specimen, which was used in most tests, had a 3/4-in. gage length and 1/4-in. gage diam. The cone-end specimen, which was used primarily to investigate the effects of a smaller gage diameter and the practicability of the modified grips and specimen, had a 3/4-in. gage length and a 1/8-in. gage diam. In both cases, the gage length terminated at 0.005-in. high shoulders which served as fiducial marks for optical strain measurements. Surface finish on the gage length was 16 µ-in. rms. Creep rates and rupture times were not significantly different for the two types of specimens and were not affected by electropolishing the specimens before testing. TESTING PROCEDURE The constant-load creep-testing machine used has been described by Smith, Olson, and Brown.5 In it the specimen is held vertically by grips of similar material and on the axis of a cylindrical tungsten or tantalum heater-tube. The specimen is loaded by means of the specimen grips, a pull rod (which is sealed to the chamber lid by a vacuum-tight bellows), a mechanical lever system, and hanging dead weights. Both specimen and grips are heated by radiation from the heater-tube, which is heated by its own electrical resistance. An optical system views the incandescent specimen through slits in the radiation shielding and heater-tube. The optical system projects an enlarged image of the specimen gage length on a ground-glass screen. Periodic gage-length measurements are made on this image with two cathetometers. Thorium oxide coatings on the specimen threads or conical end surfaces completely prevented diffusion-welding of specimens to grips, and were used

Jan 1, 1960