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By Paul L. Russell

THIS is a progress report of an experiment being undertaken in cooperation with the Bethlehem Steel Corp., the Crucible Steel Co., and the Rock Bit Sales and Service Co., involving heat treatment of the shank ends of drill steel. This experiment is being conducted by the U. S. Bureau of Mines in its experimental mine, Mining Research Branch, Bluemont, Va. The purpose of the experiment is to determine the effect of an increase in the time the steel soaks in the furnace during the hardening heat. It has been thought that increasing this time produces a soft zone below the lugs resulting in a metallurgical notch that causes early failure. Each of the steel companies furnished enough 11/4 - in. straight carbon, hollow, round steel to make up 10 sets of drill steel, in each instance the steel bars were from the same heat. These sets of drill steel, consisting of 2-ft, 4-ft, 6-ft, and 8-ft lengths were fabricated by the Rock Bit Sales and Service Co. Special attention was given to the forging of the steel to produce the best rods possible. The heat treatment of all thread ends was identical and followed the best practice. The heat treatment of the shank ends of five sets of steel from each company produced a soft zone 2 to 4 in. in front of the lugs. It was decided that possibly the best way to obtain this effect was not to overlap the hardening heat but to let the steel soak for an additional 30 min before quenching. Therefore the only variable in the test steels is the length of time the shank ends were in the furnace. The remaining drill steel shanks were treated as follows: Heat treatment in pyrometer-controlled furnace at 1550°F. Quenching oil at 105°F to 125°F temperature. Areas for heat treatment were; shanks, 11 in.; threads, 9 in. Time at heat, standard practice, 20 min for 11/4-in. steel. Actual drilling tests were made in greenstone, (a metamorphosed basaltic rock), and in epidosite. Greenstone has a specific gravity of 2.96 and a compressive strength of 44,200 psi. Epidosite has a specific gravity of 3.26 and a compressive strength of 63,100 psi. All drilling tests were made using a 31/2-in. column-mounted, automatic feed drifter, with a controlled air pressure of 90 psi at the throttle. Tungsten-carbide bits of 2 in. diameter were used for all drilling. Contrary to expectations the drill steels that were allowed to soak for the additional 30 min before quenching performed better than the steels that were heat treated according to standard practice. This performance, as shown in Table I, was especially noticeable in the drilling of epidosite. The "longheat" drill steels furnished by Company "A" drilled 154 pct more minutes than the "standard-heat" steel. Expressed in feet, the "long-heat" steel drilled 114.60 ft more before failure than the "standard-heat" steel. The "long-heat" steel furnished by Company "B" drilled 37 pet more minutes or 60.39 ft more before failure than the "standard-heat" drill steel. The effect of the long heat treatment was not as evident when the steels were drilling in greenstone (Table II). In greenstone, the increase in minutes drilled by the "long-heat" steel over the "standard-heat" steel was 47 pet and 1 pet, respectively, for Companies "A" and "B."

Jan 1, 1952

By Clyde E. Williams, JAMES L. GREGG

THIS review of the past year's progress in iron and steel metallurgy presents examples of only a few of the interesting or important accomplishments made in the United States. In the field of iron ore concentration increased attention was given to the study of the more difficultly separated wash ores and some progress was made in tabling. One difficulty with the table, in concentrating iron ore where the percentage of concentrate in the feed is large, has been the removal of fine silica from the thick layer .of concentrates in the cleaning zone. One company has -Made an important contribution toward the solution of this problem by an extension of the well-known plateau principle. By a special riffling of the plateau section of the table, the concentrates are crowded together. This action forces the fine silica to the top of the bed in the cleaning zone, whence the cross-flowing currents of water -can wash it into the middling product. Some work has been done on the application of froth flotation to the concentration of iron ores. Laboratory experiments were made at the Colorado School of Mines in which hematite was, successfully floated. Using oleic acid as a frothing and collecting agent and sodium carbonate as the conditioning agent, a high recovery of rich ,concentrate was obtained. A laboratory flotation unit is in use at Taconite, on the Mesabi range, and a commer-

Jan 1, 1932

By M. A. Grossman

The harden ability of most steels can be predicted within 10 to I5 per cent provided the complete chemical composition is known, including "incidental" elements; and provided the as-quenched grain size is known; and provided, finally, that the composition and heating temperatures for hardening are such as to result in austenite free from carbide particles. In the method proposed herein, the steel is considered as having a base hardenability due to its carbon content alone (the hardenability of a "pure steel" of the given carbon content, without any other elements), and this base hardenability is multiplied by a multiplying factor for each chemical element present. After multiplying all these together, the final product is the hardenability. Grain size may be taken into account either in the base hardenability or after the multiplication. Hardenability is stated in terms of "ideal critical diameter", namely, the diameter of bar, in inches, that will just harden all the way through (absence of un-hardened core) in an "ideal" quench, and the calculation may also be related to the Jominy test The data bring out certain features rather clearly. For example: i. It is quite useless to attempt to predict hardenability unless all elements, including "incidentals,,) are known; thus an "incidental,, chromium content of 0.20 per cent increases the hardenability by about 50 per cent. 2. The relative effectiveness of different alloys is sometimes unexpected; thus molybdenum when calculated in this way appears to be of the same order of effectiveness as manganese, rather than much more powerful, as would appear to be common experience; observe that an increase from no manaanese to 0.20 per cent Mn provides a multiplying factor of 1.67, and an increase from no molybdenum to 0.20 per cent Mo provides a factor of 1.63, an increase of over 60 per cent in each case. However, if to a steel containing 0.50 per cent Mn there is added "20 points of manganese," the factor is raised from 2.65 (for 0.50 per cent Mn) to 3.35 (for 0.70 per cent Mn), or an increase of only 26 per cent. Thus the fist small addition of an element has a much more powerful percentage effect than an equal further addition when some is already present, and in most cases the effect of molybdenum is considered in relation to a steel in which molybdenum is absent. 3. If two elements are equally effective, a greater hardenability will be obtained by using, for example, 0.5 per cent of each than by using I.o per cent of either of them alone. 4. A knowledge of the as-quenched grain size is essential for precise work, since a difference of only one grain size number (say No. 7 instead of No. 6) makes a difference of almost 10 per cent in hardenability (in these units); this, however, does not apply to certain It should be emphasized that in chromium steels (over 0.30 per cent Cr) and chrome-molybdenum and chrome-vanadium steels, un-dissolved carbides are likely to be present in the steel as quenched, and that in such cases the charts can indicate only a maximum Passible hardenability, whereas the extent of hardening actually obtained may be much less. Thus tests on a number of chrome-molybdenum steels have indicated a degree of hardening amounting to only 50 to 65 per cent of the maximum possible, and in chromium steels from full hardening (100 per cent) down to as low as 70 per cent. On the other hand, when the amount of such elements is small (Cr under 0.30 per cent, Mo up to 0.25 per cent in the

Jan 1, 1942

By M. A. Grossman

The harden ability of most steels can be predicted within 10 to I5 per cent provided the complete chemical composition is known, including "incidental" elements; and provided the as-quenched grain size is known; and provided, finally, that the composition and heating temperatures for hardening are such as to result in austenite free from carbide particles. In the method proposed herein, the steel is considered as having a base hardenability due to its carbon content alone (the hardenability of a "pure steel" of the given carbon content, without any other elements), and this base hardenability is multiplied by a multiplying factor for each chemical element present. After multiplying all these together, the final product is the hardenability. Grain size may be taken into account either in the base hardenability or after the multiplication. Hardenability is stated in terms of "ideal critical diameter", namely, the diameter of bar, in inches, that will just harden all the way through (absence of un-hardened core) in an "ideal" quench, and the calculation may also be related to the Jominy test The data bring out certain features rather clearly. For example: i. It is quite useless to attempt to predict hardenability unless all elements, including "incidentals,,) are known; thus an "incidental,, chromium content of 0.20 per cent increases the hardenability by about 50 per cent. 2. The relative effectiveness of different alloys is sometimes unexpected; thus molybdenum when calculated in this way appears to be of the same order of effectiveness as manganese, rather than much more powerful, as would appear to be common experience; observe that an increase from no manaanese to 0.20 per cent Mn provides a multiplying factor of 1.67, and an increase from no molybdenum to 0.20 per cent Mo provides a factor of 1.63, an increase of over 60 per cent in each case. However, if to a steel containing 0.50 per cent Mn there is added "20 points of manganese," the factor is raised from 2.65 (for 0.50 per cent Mn) to 3.35 (for 0.70 per cent Mn), or an increase of only 26 per cent. Thus the fist small addition of an element has a much more powerful percentage effect than an equal further addition when some is already present, and in most cases the effect of molybdenum is considered in relation to a steel in which molybdenum is absent. 3. If two elements are equally effective, a greater hardenability will be obtained by using, for example, 0.5 per cent of each than by using I.o per cent of either of them alone. 4. A knowledge of the as-quenched grain size is essential for precise work, since a difference of only one grain size number (say No. 7 instead of No. 6) makes a difference of almost 10 per cent in hardenability (in these units); this, however, does not apply to certain It should be emphasized that in chromium steels (over 0.30 per cent Cr) and chrome-molybdenum and chrome-vanadium steels, un-dissolved carbides are likely to be present in the steel as quenched, and that in such cases the charts can indicate only a maximum Passible hardenability, whereas the extent of hardening actually obtained may be much less. Thus tests on a number of chrome-molybdenum steels have indicated a degree of hardening amounting to only 50 to 65 per cent of the maximum possible, and in chromium steels from full hardening (100 per cent) down to as low as 70 per cent. On the other hand, when the amount of such elements is small (Cr under 0.30 per cent, Mo up to 0.25 per cent in the

Jan 1, 1942

By C. O. Lee, R. H. Feierabend, Z. W. Bartlett

DESPITE the fact that American brimstone production has increased 2 times since the prewar period 1935-1939, the demand for sulphur exceeds the supply. To alleviate this situation efforts are being made to increase the production of sulphur and bring the shortage to an end. The most important developments are being undertaken on the Gulf Coast. One new brimstone mine has been put into operation and three others are being developed. These projects are expected to account for a large part of the additional sulphur production now anticipated for the free world.'.' Except for a small amount of byproduct sulphur from sour natural gas and refinery gases, American brimstone is produced by the same process devised by Frasch 60 years ago, consisting essentially of the injection of superheated water at about 325°F into sulphur-bearing formations through wells which are drilled from the surface by standard oilfield methods. Sulphur deposits vary in depth from a few hundred feet to 2500 ft from the surface; in a typical deposit the sulphur occurs as crystalline aggregates in porous limestone and gypsum in concentrations varying from 5 to 40 pct, the thickness of the formation ranging from a few feet to several hundred.3 The deposits are usually surrounded by formations impermeable to the flow of hot water, the top and sides being enclosed by impermeable sediments and the bottom by dense impermeable anhydrite. As the hot water leaves the well bore, it percolates through the formation and transmits its heat to the rock and sulphur. When the sulphur reaches 240°F it melts, separates from the rock, and flows through the hot channels downward to the bottom of the well. Here it is freed from incoming water and from formation water, which saturates the porous rock, by gravity separation, liquid sulphur being 1.8 times as heavy as water. It then is pumped to the surface in a relatively pure state, 99.5 pct or better. Chief contaminants are organic impurities, such as petroleum residues, which are soluble in sulphur and tend to discolor it.' Sixteen deposits of commercial magnitude have been discovered in the Gulf Coast area. Five of these deposits have been depleted and abandoned with production totalling more than 26,886,000 tons. Eight properties are operating and have produced 65,875,-000 tons to Jan. 1, 1952, for a total Frasch-type production of 92,761,000 tons. Three new deposits are under development. Aforementioned deposits are listed in Table I. Each of these deposits has been found in the cap-rock overlying shallow intrusive salt plugs or domes and buried in several hundred to as much as 2500 ft of sediments. All salt domes do .not contain sulphur; only 16 sulphur deposits have been found in a total of 231 salt domes which are known to exist in the Gulf Coastal states of Texas, Louisiana, Mississippi, and Alabama. Ten of the salt domes lie in the Gulf of Mexico offshore from the Texas and Louisiana coasts. Additional offshore domes may be found, but their value as a sulphur potential is questionable owing to the great hazard and high cost that can be visualized at these exposed locations where depths of water reach 50 ft. Marsh operations of Freeport Sulphur Co. are in the southeast section of Louisiana. In general, the country is low, flat, relatively uninhabited marshland broken by many shallow lakes and bayous which extend for irregular distances inland. Geologically, the coastal area is of sedimentary origin, having been built up gradually under the sea by deposition of material carried down by large streams to their deltas. Offshore bars were formed enclosing

Jan 1, 1953

By C. O. Lee, Z. W. Bartlett, R. H. Feierabend

DESPITE the fact that American brimstone production has increased 2 times since the prewar period 1935-1939, the demand for sulphur exceeds the supply. To alleviate this situation efforts are being made to increase the production of sulphur and bring the shortage to an end. The most important developments are being undertaken on the Gulf Coast. One new brimstone mine has been put into operation and three others are being developed. These projects are expected to account for a large part of the additional sulphur production now anticipated for the free world.'.' Except for a small amount of byproduct sulphur from sour natural gas and refinery gases, American brimstone is produced by the same process devised by Frasch 60 years ago, consisting essentially of the injection of superheated water at about 325°F into sulphur-bearing formations through wells which are drilled from the surface by standard oilfield methods. Sulphur deposits vary in depth from a few hundred feet to 2500 ft from the surface; in a typical deposit the sulphur occurs as crystalline aggregates in porous limestone and gypsum in concentrations varying from 5 to 40 pct, the thickness of the formation ranging from a few feet to several hundred.3 The deposits are usually surrounded by formations impermeable to the flow of hot water, the top and sides being enclosed by impermeable sediments and the bottom by dense impermeable anhydrite. As the hot water leaves the well bore, it percolates through the formation and transmits its heat to the rock and sulphur. When the sulphur reaches 240°F it melts, separates from the rock, and flows through the hot channels downward to the bottom of the well. Here it is freed from incoming water and from formation water, which saturates the porous rock, by gravity separation, liquid sulphur being 1.8 times as heavy as water. It then is pumped to the surface in a relatively pure state, 99.5 pct or better. Chief contaminants are organic impurities, such as petroleum residues, which are soluble in sulphur and tend to discolor it.' Sixteen deposits of commercial magnitude have been discovered in the Gulf Coast area. Five of these deposits have been depleted and abandoned with production totalling more than 26,886,000 tons. Eight properties are operating and have produced 65,875,-000 tons to Jan. 1, 1952, for a total Frasch-type production of 92,761,000 tons. Three new deposits are under development. Aforementioned deposits are listed in Table I. Each of these deposits has been found in the cap-rock overlying shallow intrusive salt plugs or domes and buried in several hundred to as much as 2500 ft of sediments. All salt domes do .not contain sulphur; only 16 sulphur deposits have been found in a total of 231 salt domes which are known to exist in the Gulf Coastal states of Texas, Louisiana, Mississippi, and Alabama. Ten of the salt domes lie in the Gulf of Mexico offshore from the Texas and Louisiana coasts. Additional offshore domes may be found, but their value as a sulphur potential is questionable owing to the great hazard and high cost that can be visualized at these exposed locations where depths of water reach 50 ft. Marsh operations of Freeport Sulphur Co. are in the southeast section of Louisiana. In general, the country is low, flat, relatively uninhabited marshland broken by many shallow lakes and bayous which extend for irregular distances inland. Geologically, the coastal area is of sedimentary origin, having been built up gradually under the sea by deposition of material carried down by large streams to their deltas. Offshore bars were formed enclosing

Jan 1, 1953

By R. W. Armstrong, D. H. Feisel

Self-diffusion in pure crystalline solids has been described through extension of the Cohen and Tum-hull volume -fluctuation model originally proposed for diffusion in simple liquids. It is shown, for a number of crystalline solids, that the self-diffusion coefficient, D, obeys the relationship where a is the lattice spacing, v the Debye frequency, Z' the lattice-volume fluctuation per atom required for a diffusion jump, and (?V/Vo) the relative increase in the lattice volume resulting from thermal expansion between O°K and the temperature under consideration. The calculated value of Z' is dependent upon the difiusion mechanism and the lattice geometry. ThE need for an increased understanding of mass-transport processes in crystalline solids has resulted in much research to determine rates of self-diffusion.' For several metals (e.g., copper, silver, and iron), the experimental values of the self-diffusion coefficient, D, have been determined over a large interval of temperature and the accuracy of D has been investigated through repeated experiments. Also, a number of empirical and theoretical diffusion studies have established a rational basis for understanding the D values for the different elements.2"6 The empirical diffusion analysis by Sherby and simnad6 supplied the main stimulus for the present study. Sherby and Simnad, reviewing the self-diffusion data for a substantial number of pure crystalline solids, suggested that sufficient data were available to establish with some certainty the apparent intrinsic material properties which influence D. Without explicit regard for any mechanism of diffusion, these investigators obtained an empirical relationship for D which correlated the self- diffusion coefficient for each element with the melting temperature, crystal structure, and valence of the particular element. Their analysis is only unsatisfactory in that the effect on D of crystal structure is not very clear and the valence to be assigned to an element is not always straightforward. The present study is an attempt, from a very different viewpoint from that of Sherby and Simnad, to establish a basis for understanding the self-diffusion coefficients for crystalline solids. This analysis was undertaken for the purpose of developing a general expression for D which would explicitly depend on the mechanism of diffusion. The main result of the study is that diffusion in crystalline solids may be described in terms of a volume-fluctuation model which was originally proposed by Cohen and Turnbull7 to describe diffusion in simple liquids. The model appears to be useful for predicting self-diffusion coefficients in crystals. The following sections describe the volume-fluctuation model for diffusion, the application of this model to crystals, and the resultant agreement with experimental data. 1) THE VOLUME-FLUCTUATION MODEL FOR DIFFUSION Cohen and Turnbull7'8 developed their model for liquid self-diffusivity for the purpose of describing certain properties of liquids, glasses, and the liquid-glass transition. A hard-sphere model for the liquid structure is used. In this model, the size of a spherical molecule or atom is fixed for all temperatures by the interatomic spacing at the absolute zero of temperature. At any temperature above O°K, the atom is viewed as being contained within a larger spherical cage defined by the interatomic spacing of the atoms at that temperature. A random distribution of varying cage sizes is assumed to exist in the liquid. An individual diffusion jump occurs when the free volume of an atom (the volume of the cage containing the atom minus the volume of the atom) is large enough for the atom to jump out of its cage. With this physical picture of diffusion in liquids, Cohen and Turnbull derive the following equation for self-diffusivity: D=Doe-yv*/vf [1] where Do is the product of three factors which are the diffusion-path geometry, the diffusion-jump distance, and the velocity of the diffusing atom, v*

Jan 1, 1964

By M. A. Cook

Sutherland used an ion-pair adsorption model to derive the author's hy-drolytic pee-acid) adsorption equation for the contact bubble curves of Wark and Cox. To do so it was necessary to postulate that the sum of coverages of surface anion sites by the collector and depressant anions is practically unity. It is here shown that the free energy of Sutherland's postulated collector ion (x-)-depressant ion (OH-) exchange reaction (for no other than the OH- to compete with X-), namely EX + (OH-) Z SOH- + X-, is in some cases positive and X- should not even adsorb. Also, in many cases the (OH-) adsorption must be quite negligible even though the collector covers only about a sixth of the mineral surface at the threshold of air bubble contact. This, however, contradicts the postulate that permits one to derive the correct bubble contact eqwztion for the ion-pair model. Furthermore, the requirement for charge neutrality leads in the ion-pair model to the (impossible) constancy of the ratio @+)/(OH-) along a contact bubble curve in which pH may change by more than seven units. HYDROLYTIC ADSORPTION EQUATION Hydrolytic (free-acid or free-base) and ion-pair (H', X-, or R', OH-) adsorption models of the collector in metal sulfide and similar flotation systems are superficially alike and somewhat difficult to differentiate. This is because they yield, under seemingly valid assumptions, equivalent forms of the equations describing the distribution of the collector between the aqueous solution and the mineral surface. This has been discussed by the author and associates1-4 and more recently by Sutherland,' both for simple collector-mineral and for more complicated collector-depressant-mineral systems. In the hydrolytic adsorption model the equations describing the contact bubble curves of Wark and coxeJ7 are as follows :2 Here X is the collector anion, D- the depressant anion, 9, and On are the fractions of the free-acid sites S on the surface of the mineral covered by collector and depressant free acids, respectively, and @ is the fraction of uncovered sites. Kx is the free-acid collector dissociation equilibrium con- stant, K1 that for the free-acid collector adsorption, KD that for the free-acid depressant dissociation, and K2 the equilibrium constant for the free-acid depressant adsorption. Eqs. 1 to 5 yield upon simultaneous solution the result is the critical free-acid concentration for bubble contact in the absence of depressant-free acid. Eq. 8 expresses the conditions along a simple collector-mineral contact bubble curve for the case HD = 0, or V = 0. Last and Cook showed that Eq. 6 applies generally and with good accuracy in the collector-depressant-metal sulfide mineral systems. Inci-dentally, it has been shown by infrared absorption studies that in some cases the free-acid adsorption process splits out water.' In this case, Eq. 2 might be written SHOH + HX Z SHX + H20, with a similar equation replacing Eq. 4 for depressant-free acid-water exchange. This possibility does not change, however, the basic equations or considerations of the hydrolytic adsorption model. Indeed, this type of free acid-water exchange reaction was predicted for fluorite and iron ore flotation by oleic acid in the dry grinding and boiling processes.410

Jan 1, 1961

By H. H. Waller, D. L. Monroe, D. P. R. Smyth

ORIGINALLY slusher drift development was conventional, advancing the drift full 10x13-ft size at 6 ft per round. This proved dangerous and costly because the weak fractured rock of the orebody cannot be left raw for any length of time without its reacting with air to cause spalling. With this method of drift development ground conditions were worsened by many blasts and the length of time it was necessary for the drift to remain open. The problem was practically solved by driving 5x7-ft pilot drifts, then enlarging to 10x13-ft raw size by slashing with 50 to 60-ft diamond drill holes. Calculated explosive charges are used to avoid wall and roof shattering. Still more recently jacklegs and sectional steel replaced the diamond drills, resulting in the same work for less than half the cost, see Figs. 1 and 2. Crosscuts at right angles to the main haulage drifts, which cross through the center of the ore-body, divide the ore into 200-ft blocks. Eight slusher drifts on 50-ft centers draw from one block. The slusher floor is 11 ft above the rail, inclined at 1 pct grade, and the top is 18 ft below the undercut. The finished slusher drift is 102.5 or 120 ft long, depending on whether it is north or south of the crosscut. Drawpoints are staggered on each side at 17.5-ft centers. The completed drift is concreted and has an inclined ramp and a vent at the back. When crosscuts and gangways have been excavated and concreted and slusher stations installed, slusher drift development is carried out in 10 clear-cut stages: 1—Pilot drift is driven full length, 5x7 ft. 2—Station is excavated at half-way point in pilot drift. 3—Pilot drift is enlarged to slusher drift size by drilling. 4—Lower part of slash is blasted and mucked for floor concrete. 5—Floor is poured. 6—Inside upper half of slusher drift is blasted, mucked, and concreted. 7—Outside upper half of slusher drift is blasted, mucked, and concreted. 8—Drawpoints are excavated. 9—Drawpoints are concreted. 10—Concrete ramp and sheave protection recess are constructed at back end of slusher drift. A 5x7-ft pilot drift is driven full length on the center line of the proposed slusher drift using a jackleg and detachable bits on 7/8-in. hexagon steel. A 10-hp air-driven slusher and 36-in. scraper pull muck directly into cars in the main haulage crosscut, see Fig. 2. Operations are on a three-shift basis. One man mucks the previous round, drills, and blasts his round in a shift. Average advance is 5 ft per shift. When the pilot drift is completed, 7 ft of drift in the center section is enlarged to full raw slusher drift size of 10x13 ft, for the set-up to drill long slash holes. The pilot drift is slashed to full raw size from this station with jacklegs and tungsten carbide chisel bits on 7/8-in. sectional steel. Crews line the holes without trouble, working from controls established by the engineers, and the pattern of holes for the slash is arranged to give the least shattering effect

Jan 1, 1955

By J. P. Boisseau, C. N. J. Wagner, E. N. Aqua

An analysis ulas made of powder-paltern peaks from cold-rolled polycrystalline copper and from copper powders, compacted into briquets (1 in. diameter) with pressures up to about 106 psi. Powder-pattern peaks from both contact faces were measured with a diffractometer and CuKa radiation. Laltice-parameter measurements indicate the presence of residual stresses in the bulk specimen of the order of a - -10 kg per sq mm after 93 pct reduction in thickness, and give some evidence for the occurrence of deformation stacking faults (probability a - 0.003) in both bulk and powder samples. Fourier analyses of the line profiles were carried out on the (111) - (222) and (200) - (400) Pairs of reflections. The particle sizes decrease rapidly with increasing deformation and reach asymptotic values of De (111) = 550A and D, (200) = 350A at about 25 pct reduction in thickness or 80,000 psi pressure for compaction. The anisotropy of the particle sizes indicates the presence of microtwins and stacking faults on (111) planes. The rms strains increase also with deformation and reach limiting values of 2 x 10-3 in the [100] direction and 1 x 10-3 in the [Ill] direction at a distance L = 100A normal to the reflecting planes. THE diffraction of X-rays in cold-worked, polycrystalline, fcc metals and alloys yields Debye-Scherrer patterns in which the individual (hkl) lines may show a broadening, a shift, and an asymmetric shape.' These effects can be explained by the fragmentation of the small, coherently diffracting domains, the presence of residual elastic strains in the lattice, and the formation of stacking faults. X-ray studies of stacking faults in fcc metals and alloys have been methodically performed during the last few years, but so far most of the investigators dealt with cold-worked powder specimens obtained by filing.2-8,10-19 In such specimens, the crystals are randomly oriented and the average elastic strains are assumed to be zero, so that the observed peak shifts are due to stacking faults only. The agreement between X-ray diffraction theory1,20 and experiment is generally good. On the contrary, cold-worked, polycrystalline bulk specimens (after wire drawing, rolling, plastic deformation by tension or compression, etc.) contain residual elastic strains, which may not average to zero in the surface of the specimen and show very strong preferred orientation of certain lattice planes (texture) parallel to the specimen surface. Nonzero elastic strains also produce peak shifts, the magnitudes of which depend upon the crystallographic orientation of the reflecting lattice planes in elastically anisotropic materials as well as on the type of plastic deformation and which have to be taken into account when measuring stacking-fault probabilities in deformed bulk specimens.21-23 The purpose of the present investigations was to perform a detailed X-ray analysis on a bulk specimen of a fcc metal deformed by rolling at room temperature and on powder of the same material deformed by compaction, and to compare these results with those previously obtained on cold-worked filings.18 Pure copper was chosen for this study since it is known to produce only a small quantity of stacking faults by filing at room temperature.3,16,17,19 The residual elastic strain in the surface of the bulk copper should be the predominant factor determining

Jan 1, 1965

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,' there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells' and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported' in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F' (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 '/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By H. NORTON JOHNSON

THE oil industry in California during 1929 reached new heights and new depths in the discovery and development of the oil resources of the State. The discovery of new fields, and more especially the discovery and development of deeper prolific sands in known fields has, for the first time in its history, brought the potential production of completed wells within the State to over 1,000,000 bbl. oil per day. Constant improvement in equipment and technique has made possible economic development to depths unheard of but a few short years ago. Commercial production from a depth of over 4000 ft. was considered quite an accomplishment in 1923 when the Meyer sand at Santa Fe Springs was developed, and when later oil was successfully raised from this depth.

Jan 1, 1930

By Brahm Prakash, R. Schuhmann

Chemical conditions for flotation and nonflotation of quartz with oleic acid as collector and barium, calcium, aluminum, iron, and tin as activators were studied using a simple vacuum-flotation technique in glass-stoppered graduates. The detailed study of barium activation led to an interpretation based on ideal Langmuirian chemisorption.

Jan 1, 1950

By R. Ruka, E. A. Gulbransen

ONE of the interesting questions in the understanding of the reaction of iron with oxygen is the kinetics and the mechanism of the crystal structure changes occurring in the formation and breakdown of the oxide film. In a recent work' the electron diffraction method was applied to the study of the solid phase reactions occurring internally in the oxide film on iron above 570°C and under vacuum conditions. The higher oxides which form under oxidizing conditions are reduced internally by the diffusion of iron into the oxide leaving the bulk of the oxide FeO (wüstite). This paper will ask and consider three questions. These are: (1) What is the nature of the depressed transformation temperature for the Fe3O4 + Fe ? 4Fe0 reaction in very thin oxide films?; (2) What is the mechanism of the forward transformation of Fe3O4 to FeO at or near 570°C?; and (3) What is the nature and mechanism of the slow reverse transformation of FeO to Fe3O4 and Fe below 570°C?. The composition of the oxide as well as its electrical, magnetic, mechanical, and chemical properties depends upon the kinetics of these reactions. Literature Survey The composition of the oxide film on pure iron at temperatures up to 570°C has been studied extensively by the electron diffraction method. Nelson,' Jackson and Quarrell,3 and Gulbransen and Hick-man4 have shown that Fe3O4 and a-Fe2O8 are formed in the temperature range of 225" to 570°C, while y-Fe,O, is most likely formed below 225°C for long oxidation times. In very thin films FeO (wüstite) is found to form at temperatures as low as 400°C, and its existence depends essentially upon the extent of initial oxidation. FeO is not found in the formation of thick films below 570°C. On the other hand X-ray5 and micrographic8 studies show that Fe3O4 may exist as the main com-ponent in thick films up to 650°C, well above the equilibrium temperature for the reaction Fe3O4 + Fe ? 4FeO. The kinetics of the forward and reverse trans-formations of the reaction Fe3O4 + Fe ? 4FeO have not been studied in oxide films. However, analysis of the data of Gulbransen and Hickman4 on the heat-ing and cooling of iron oxide films of known thick-nesses in high vacua shows that the forward reac-tion proceeds rapidly even for a 4000 A film at temperatures of 575" to 600°C. The reverse reaction or decomposition of wüstite (FeO) occurs at tem-peratures below 450°C. Thus, there appears to be a slow process in the decomposition which is in marked contrast to the rapid forward reaction. The decomposition of a bulk sample of FeO free from the metal has been studied extensively by Chaudron, Benard and coworkers using the micro-graphic, X-ray diffraction, and thermomagnetic methods. Chaudron7,8 first observed that the de-composition of FeO (wüstite) below 570°C occurs by the reaction 4FeO ? Fe3O4 + Fe. Later work by Chaudron and Forestier5 showed that the rate of de-

Jan 1, 1951

By H. M. Woodroffe, H. K. Conn, S. J. Rice

World production of asbestos is estimated to be at a current level of almost 3.5 million tons, having more than doubled in the past ten years. A substantial part of the increase has been due to a rapid expansion in the Soviet Union. Production from that country during 1964 is estimated at 1.5 million tons and, as a consequence, Russia has displaced Canada as the leading world producer. Although traditionally the asbestos mining industry has been centered near Sverdlovsk in the Urals, two new producing areas have been under development for some time. It is expected that a new mine will be in operation in 1965 near Kiembi, Kazakhstan, some 300 miles south of Sverdlovsk, and an- other mine at Aktrovak in Tannu-Tuva, west of Lake Baikal. These developments will provide a significant increase in the production capability of Russia. Although internal consumption is expected to increase with the addition of new asbestos- cement producing facilities now under construction in Russia, there is some speculation that exports will also increase.

Jan 2, 1965

By L. K. Jetter, J. C. Ogle, C. L. McHargue

The preferred orientation developed in extruded aluminum rods has been studied as a function of extrusion temperature, extrusion speed, and position in the rod. Duplex <111> - <001> textures were developed for slow extrusion speeds at temperatures of 75° to 850° F and for fast extrusion speeds at temperatures of 75° to 450°F. The <001> texture component was shown to be primarily due to re crystallization occurring during fabrication. At fast speeds and billet temperatures of 650° to 850°F, complete recrystallization occurred and <115>or<118> textures were found. The nature of the structure has proved to be an important variable in the production and use of extruded products. Data on the flow of aluminum and aluminum alloys summarized by Smith,&apos; Hardy,&apos; and Locke3 show that the extruded product may possess a deformed, a partially recrystallized, or a completely recrystallized structure, and there may be important variations in the structure from surface to center and from front end to back end of an extrusion. This inhomogeneity in grain structure and preferred orientation affects both the mechanical properties of the extruded section and its response to subsequent heat treatment. Among the fabrication variables causing these differences are temperature, extrusion ratio, and extrusion speed. Preferred orientation which develops during the extrusion of rods is of the fiber-type and, in general, has been assumed to be similar to that developed in rods or wires fabricated by drawing through dies, rolling, or swaging.4 Because of the nature of the flow of metal being extruded, this assumption may be valid for material near the center of the rod but probably is not valid for the outer layers. In most face-centered-cubic metals a duplex fiber texture has commonly been reported in which the grains have either <Ill> or <001> directions parallel to the longitudinal axis. Sachs and fichiebold5 reported cold-drawn aluminum (99.6 pct pure) to have a single <Ill> fiber texture, and this observation was confirmed by Schmid and Wassermann.6 Hibbard, on the other hand, observed a minor <001> and a major <111> texture in 99.994 pct A1 cold drawn to 98 pct reduction in diam.7 He concluded that the <001> component resulted from a small amount of room-temperature recrystallization. Dayal8 concluded that the <001> component was an intermediate component which disappeared at high reductions in 99.5 pct pure Al. Kostron and schippers9 found duplex <111> — <001> textures in extruded 99.5 pct Al, as did Gow and cahnl0 and GOW11 for extruded rods of commercial and superpure aluminum. Similar duplex fiber textures have been reported for aluminum alloys by Kostron,= Unckel,13 and Van Horn.14 The present paper is concerned with the variation in texture with fabricating conditions and with the nature of the texture components in extruded aluminum rod (99.99 pct pure). EXPERIMENTAL PROCEDURE Ingots were chill-cast in cast-iron molds and machined to 3-in. diam by 6-in. long extrusion billets. These billets were upset to 3.125 in. diam and extruded through a flat-face 0.690-in. diam die. Quenching of the rods was accomplished by a water spray at the die face. The combinations of fabricat-

Jan 1, 1960

By James P. Kimball

Jan 1, 1885

By Arne F. Westgren

X-ray analysis and single-crystal study have been utilized in recent years as a new means of following constitutional changes in alloys. If such transformations can be suppressed by rapid cooling, they can be followed at room temperature in a particularly convenient manner. In the following we shall consider changes in solubility and polymorphic transformations with particular reference to phenomena of the age-hardening type. Finally a thermodynamic viewpoint is developed for examining such transformations. Changes in Solubility 1. Determinations of solubility limits in the solid state which show decreasing solubility with falling temperature are made as follows: A series of alloys extending into the heterogeneous region is prepared and quenched fromas high a temperature as possible, whereupon their lattice parameters are determined. Then one or more alloys are quenched from temperatures at which they are heterogeneous and their lattice parameters likwwise determined. For the purpose of determining the parameter the apparatus shown in Fig. 1 has been very useful for it produces sharp films in a short time which can be accurately read. High-order reflections (interferences) from the object are recorded on a film which is placed exactly perpendicular to the X-ray beam. The specimen usually has the shape of a small round bar.l Fig. 2 shows a selection of such exposures of silver-rich Cu-Ag alloys, and Fig. 3 gives the measurements made from these films. Fig. 4 gives the solubility curve which results.2 This curve is shifted to lower concentrations than the curve that is obtained from metallographic or physical methods. The X-ray method unquestionably gives more reliable data

Jan 1, 1931

By G. T. Jackson

The Alaska Gastineau Mining Co.&apos;s mine is located at Perseverance, about 4 mi. east of Juheau, Alaska. Its property consists of a group of claims, the lode system traversing these claims for a distance of 11,000 ft. (3352 m.). It is shown in Fig. 1. The ore deposits occur in what is known as the Juneau gold belt. This gold belt can be traced for about 50 mi. northwest of Juneau and 40 mi. southeast. It consists of a single band, several hundred feet wide, in which stringers and veins of quartz, carrying gold, occur in a slate formation near its contact with some altered volcanic rock known as greenstone. The Perseverance orebody consists of stringer lodes, having a strike northwest and southeast, dipping about 60° to the northeast. These

Jan 1, 1920

By Frank Harris

THE strength of hard drawn copper wire is a question of considerable importance to both manufacturer and consumer. Unlike steel and alloy wires, in which strength is governed by both chemical and physical considerations, the high conductivity required for copper wire in the electrical industry generally precludes the possibility of obtaining tensile strength through the use of alloys. Consequently, this strength is largely a matter of the physical structure, and all factors known to affect this structure, such as rolling temperature, die contours, lubricants, drawing speeds, etc., are matters of prime importance. The experiments described here have been carried out during the past year at the Baltimore plant of the American Smelting & Refining Co., in connection with a general investigation of some of the questions mentioned above, with the object of studying the physical structure of hard drawn copper, wire and the influence of certain factors on that structure. The work has been of an exploratory nature, rather than comprehensive, but it was thought that the results might prove of sufficient general interest to warrant their publication. The bulk of the hard drawn copper wire used in places where strength is an important factor is manufactured to strict specification, based usually in the United States on that of the American Society for Testing Materials (B-1-23). This specification calls for almost as high a value of tensile strength; consistent with elongation, as it is possible practically to obtain, and only physically perfect material can be relied on to meet such a specification. Obvious defects, such as laminations produced through fins in the original rods or brittleness due to overdrawing, are usually recognized and need only passing reference. Laminations can be detected by twisting and untwisting the wire several times; they will show up on the surface in the form of fins. Fig. 1 shows a very bad example of this defect. The wire may be perfectly smooth before twisting but when such laminations are present they will readily show up under this treatment. This trouble is caused by similar defects in the original rod produced by overfills in rolling. Fig. 2 shows the cross-section of the rod from which the wire in Fig.1 was drawn.

Jan 1, 1928