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By J. W. Edington

THE Hopkinson bar has become a popular technique for the measurement of the mechanical properties of materials deformed at high strain rate. Maximum use of the equipment is made in the arrangement first used by Kolskyl in which a short compression specimen is sandwiched between two pressure bars and is loaded by a single pulse travelling through the system. The pressure bars are used both to apply the load to the specimen and as transducers to obtain continuous strain-time histories of three pulses, incident on, reflected, and transmitted by the specimen. The data measured by the pressure bars can be analyzed in terms of the stress/strain behavior of the specimen.2'3 However, one of the assumptions of the analysis of the observed pulses is that the total stress and total strain do not vary significantly from point to point within the specimen at any given instant during the deformation process. Although this assumption is generally justified for very short disc-like specimens2 the situation is uncertain for larger specimens. For example, at small plastic strains (-0.01) Hauser et al.2 have some evidence of small flucations in the total stress within the crystal during deformation, even in relatively short aluminum specimens. In addition, Karnes4 has shown that the plastic strain, and by inference strain rate, is different at each end of a compression specimen tested in a Hopkinson bar, although the length of the specimen was not specified. Recently, the mechanical properties and the dislocation substructure have been investigated in single crystals of columbium5 (length 0.25 in., diam 0.19 in.), and copper6 (length 0.5 in., diam 0.5 in.) deformed at high strain rates. As part of this research program the assumption that the plastic strain is constant throughout the specimen has been checked by measuring the total dislocation density as a function of position in the specimen. Compression specimens of the same orientations and dimensions were tested as described previously5,6 sing a split Hopkinson bar. Since any discontinuity in strain distribution is most likely to arise during the initial stages of deformation the investigation was performed on specimens deformed to plastic shear strains of 0.054 (copper) at a strain rate 1.2 x l03 sec-1, and 0.06 (columbium) at a strain rate 1.5 X l03 sec-1. The orientation of the single crystals is shown in Figs. 1 and 3. Thin foils were taken parallel to the most highly stressed slip plane, i.e., (111) in copper and (011) in columbium, using conventional disc techniques. The dislocation densities were measured using first order reflections with compensation for invisible dislocations.5'6 In the copper single crystals the discs were randomly distributed throughout the cross section of the specimen. However, the dislocation density obtained from each disc was plotted vs the disc positions relative to the ends of the specimen. The results for the copper specimens are shown in Fig. 1. Clearly the dislocation density is constant throughout the main portion of specimen within the experimental error. The error bars on the dislocation densities correspond to a shear strain variation of 0.015 on the basis of previous measurements% ± of the rate of increase of dislocation density with strain in copper single crystals of the same geometry. Thus within this experimental error the plastic strain can be concluded to be constant within the specimen and the assumptions used in the analysis of the stress/time curves are therefore reasonably valid. The higher measured dslocation density near the impact end and the lower dislocation density at the bar end of the copper specimen is in agreement with the results of Karnes4 who showed that this strain/time curve rose to a maximum more rapidly at the impact end compared with the bar end. Hauser et al.2 have also pointed out that at small plastic strains (-0.01) the strain at the impact end of the specimen may be greater than that at the bar end. Thin foils taken from different points within the columbium single crystals demonstrated that the dislocation density could vary significantly within the specimen, see Fig. 2. Large areas of some thin foils up to 30 µ sq contained very few dislocations, see Fig. 2(a). However, in other parts of the compression specimen dislocation configurations like those shown in Fig. 2(b) existed over large areas (-30 µ sq). As a result, when the average dislocation density in a thin foil is plotted as a function of the position of the thin foil relative to the ends of the specimen, considerable scatter is observed, see Fig. 3. In this material then, the local dislocation density, and consequently the

Jan 1, 1970

By H. T. Green, R. M. Brick

True stress-strain data on alloys of pure iron with up to 2.4 pct Al were obtained in the temperature range +100° to —185°C. Alumi-num was found to reduce yield and flow stresses of iron at low temperatures but to have little or no effect on ductility. The effects of temperature and composition on strain hardening are discussed. SEVERAL independent studies of the behavior of high purity iron binary alloys at low temperatures are now in progress in attempts to evaluate systematically the variables affecting the low temperature brittleness of ferritic steels. This paper reports the results of one such investigation in which the tensile properties of aluminum and aluminum plus silicon ferrites were measured from 100" to —192°C. True stress-natural strain data have been obtained in order to evaluate as many as possible of the parameters which describe the behavior of the materials involved. In comparable studies at the National Physical Laboratory in England, iron and iron alloys of high purity have been produced' and tested at subat-mospheric temperatures.' True stress-natural strain curves were obtained there also. The purest iron contained 0.0025 pct C and 0.001 pct O and N. Even this, as normalized at 950°C following hot rolling, showed little ductility at -196°C. The grain size was ASTM No. 3, and the room-temperature yield strength was 17,800 psi (which seems too high for pure iron). Some of the NPL irons contained considerably more oxygen and demonstrated intergran-ular fracture at —196°C. The authors2 carefully differentiated between intergranular fractures associated with excessive oxygen content and transcrys-talline cleavage with little ductility encountered at —196°C in the purer material. The cleavage stress was half again as great as that associated with inter-granular fracture. Test Material, Preparation, and Procedures Of a number of Fe-A1 alloys produced, eight were considered to be sufficiently pure for testing. Partial chemical analyses (Table I), low observed yield points, and high ductilities indicate these alloys to be comparatively pure for vacuum-melted irons of sizable ingots, 5 Ib or more. To produce the binary Fe-A1 alloys, electrolytic iron was melted in air, cast into slabs, and rolled to strips 0.010 in. thick. These strips, joined into a continuous ribbon and wound into 2 1/2 in. diameter spools, were subjected for four weeks to a moving atmosphere of purified dry hydrogen in a stainless-steel tube at 1050" to 1150°C. Charges of these spools were melted in beryllia crucibles under good vacuums (1 micron), and aluminum (99.97 pct Al) was added to the melts. Compositions of these alloys are recorded in Table I. The ingots were hot forged and then cold rolled at least 65 pct to 3/8 in. rods which were vacuum annealed to the desired grain size, approximately ASTM No. 4, prior to machining into tensile test bars. All tensile specimens had gage sections 1 in. long, with a fillet of 1.5 in. radius to the shoulder. Gage diameters were 0.250 in, except for a few rods where additional cold work required use of a 0.200 in. gage section. After machining, 0.002 in. was removed from the gage diameter using 240, 400, and 600-grit metallo-graphic papers. The final polish with 600 grit left the fine scratches running in the longitudinal direction. By this means, surface metal strained during machining was removed. A few specimens heat treated after machining were similarly reduced 0.004 in. to remove any material affected chemically by the atmosphere during heat treatments, as is discussed in a later section. Tensile tests of the eight alloys at constant temperatures from +100° to —185°C were performed in apparatus which has been described." The essentials include a double-walled insulated metal vessel which contained the liquid heat-transfer medium surrounding the test specimen. A constant temperature was maintained by means of a pyrometer which regulated the pressure of dry air driving liquid air through a copper coil. Temperature variation was less than ±2°C during a specific test. For axial straining, two lengths of case-hardened chain, terminating in simple shackles, loaded the specimen through threaded grips. The lower grip bar passed through a hole in the bottom of the test vessel to which it was joined by a thin-walled

Jan 1, 1955

By D. K. Atwood

Experiments resulted in a satisfactory laboratory method for restoring permeability to clay-containing cores damaged by fresh water. Clay contents of a number of field cores were measured, and permeabilities of plugs from these same cores were then deliberately reduced with fresh water. This damage is attributed to swollen and dispersed clays occupying the pore space. After damaging, a number of experiments were performed to meaJure the amount of damage and to establish some means by which permeability could be restored. The experiments included flooding the damaged cores with water-miscible fluids such as salt water, acetone, isopropyl alcohol and ethanol. Permeability was not successfully restored in these experiments. However, part of the damage was repaired by flooding with oil; when water was removed by distillation in the presence of immiscible fluids such as air or toluene, permeability was completely restored. This evidence suggested that swollen and dispersed clays could be collapsed to their original volume by strong interfacial and capillary forces. It was further postulated that the required forces could be generated by flooding the damaged cores with a solvent partially miscible with water. The flooding experiments were repeated using n-hex-an01 as the partially miscible solvent. Permeability was restored to five of six damaged cores and substantially increased in the sixth. A large fraction of the restored permeability was retained even after water saturation was raised to its original value with 12 per cent salt water. INTRODUCTION Sharp reductions in permeability often occur when relatively fresh water contacts clay-containing formations during drilling and workover operations. These permeability losses are caused by removing inorganic ions from the environment surrounding the clay, and consequent swelling and/or dispersion of clay minerals into the available pore space.' This phenomenon is generally termed clay damage, fresh-water damage, or simply formation damage; it causes large losses in current revenue by preventing oil wells from making their allowable production. Attempts to repair the damage and restore permeability by flowing salt water solutions or brines through clay-damaged cores containing montmorillonite have been unsuccessful.' This irreversibility is thought to result from formation of brush-heap, or edge-to-face, structures when the dispersed clay is flocculated. The brush-heap structures occupy much more space than the close packed domains present before damage.' One solution of the problem is to destroy the clay-water brush-heap and thus restore permeability. Because no satisfactory method existed for restoring permeability to clay-containing formations damaged by fresh water, the work described in this paper was under taken. The laboratory experiments generally consisted of deliberately damaging fresh cores containing clay and then attempting to repair this damage by various means. Results indicate that generating strong interfacial forces within the pore space of damaged cores collapses the clay brush-heap and restores permeability. These forces are most conveniently generated by flowing partially water-miscible solvents, such as n-hexanol, through a core. THEORY OF THE DAMAGE PROCESS The most common clay mineral groups known to cause permeability damage to formations are the mont-morillonites, kaolins, chlorites and illites. These clays are constructed of particles which can adsorb water on their surfaces and edges and, in the case of montmorillonite, between layers of the basic particle itself. This adsorption increases as water salinity decreases. At low salinities the particles disperse into the aqueous phase. When the clays present in the formation are kaolin, chlorite and illite, dispersion accounts completely for permeability damage to porous media. However, unlike the other clays, montmorillonite particles can imbibe water and adsorb ions between layers of sub-particles, or platelets. These platelets have net negative charges on their faces and are held together by exchangeable (or removable) cations such as Na and Ca decrease in ion concentration (salinity) in the fluid surrounding a particle causes migration of water into the clay layers and disperses the basic particle, while diffusion removes the original exchangeable ions from between the platelets. Once these ions are removed, the facing negative platelets repel each other, causing the montmorillonite to swell until, for all practical purposes, the individual platelets are dispersed. For this reason, fresh-water* damage is much more severe in sands containing montmorillonite than it is in sands containing other clays. Many investigators have shown that even trace amounts of montmorillonite can be responsible for marked reduction in the permeability of reservoir sands in the presence of fresh water." ." Monaghan and others have shown that fresh-water damage in montmorillonite-containing cores cannot be

Jan 1, 1965

By G. Sachs, A. W. Dana, C. C. Chow

A great number of the investigations on the plastic flow of metals have been concerned with the establishment of a "universal" stress-strain relation. In such a relation some stress function when plotted against a strain function should yield identical curves for the various stress states. In the first investigation of this type, Ludwik and Scheu1 plotted the maximum shearing stress as a function of the maximum principal strain. Later Ros and Eichinger2 introduced two universal stress-strain relations, the one relating the maximum shearing stress to the maximum shearing strain, and the other relating a stress invariant, suggested by von Mises and Haigh, to the corresponding strain invariant. (In more recent investigations the stress and strain invariants are frequently supplemented with some factor to render their meaning more lucid.) A further suggestion which has not attracted appreciable attention is that by Baranski³ who used stress and strain deviators. The most common means of experimentation to determine the relation between stress and strain consists in subjecting thin walled tubes to combined internal pressure and axial tension.4a,4b,4c This method allows the study of plastic flow under stresses which are variable in two directions. However, the plastic flow which can be obtained in this manner is comparatively small, being limited by either tension failure or instability. For copper,'. only the relation between maximum shearing stress and maximum shearing strain yielded good agreement. On the other hand, tests on a stee14b and on an aluminum alloy4c. resulted in systematic deviations if any of the discussed universal stress-strain relations were used. It would seem, therefore, that the agreement mentioned above for copper is only incidental and explained by its high rate of strain hardening compared to that of other metals. Much larger strains than experienced in the tube tests can be obtained by subjecting a thin membrane of a ductile metal, which is restrained at its periphery, to a uniform hydraulic pressure. The thin sheet forms a deep bulge before it fails. The stresses and strains in such a bulge increase with increasing distance from the edge of the clamping "die," the maximum stresses and strains occurring at the pole (crown) of the bulge. While the stress and strain states are determined by the contour of the bulge, the absolute magnitude of the stresses and strains depends upon the hydraulic pressure. The bulge contour is in turn correlated with the geometry of the die opening. The deformation and fracture characteristics of circular bulges, that is, bulges formed with circular clamping dies, have been the subject of numerous experimental and analytical investi-gations.5,6,7 It has been shown that plastically deformed circular bulges develop large and comparatively uniform strains before failure by instability"6b,6c,6d and closely assume a spherical shape.6d Also the distribution of strains across the contour of the bulge is dependent on the metal being investigated and is correlated with, but cannot be predicted from, the metal's stress-strain characteristics. On the other hand, oblong or elliptical bulges, that is, bulges formed with elliptical clamping dies, are not as susceptible to analytical analysis and have not been investigated to the extent that circular bulges have. The few available data6c,7c indicate that stress states are obtained at the poles of the bulges, varying between plane strain and balanced biaxial tension, depending upon the geometry of the die opening. In this paper, the strain state and curvatures exhibited by three bulge shapes, a circular and two elliptical bulges, Fig 1, are analyzed experimentally using methods described in previous publications.6a,6c An attempt is made to derive the stress-strain relations for these bulges, which represent strain states in which the ratio of the two positive principal strains varied between 1.0 and 0.35. In addition, tension tests yielded data for a value of —0.5 for this strain ratio. Such an analysis should indicate the applicability of the various laws correlating stress with strain to the stress and strain states occurring in bulged shapes. Definitions and Nomenclature The definitions of the major stress and strain quantities used in this paper are as follows: s1, s2, s3 = principal normal stresses Sl > s2 > S3 t = shear stress e = conventional (unit) strain e = In (1 + e) El, E2, E3 = principal natural strains 7 = shear strain The maximum shear stress: , _ S1 — S3 lmax = 2 Frequently, the flow stress, s1 — s3 = 2lmax rather than the maximum shear stress is used.

Jan 1, 1950

By G. W. Binkley, R. E. Collins, G. K. Dumbauld

A mathematical analysis has shown that the primary factors affecting the deposition of cement in unfractured perforations during squeeze-cementing operations are: the properties of the cement slurry, the geometry of the perforations, and the filtration time. The validity of the analysis has been substantiated by laboratory investigations. The information presented in this paper makes possible the prediction of the rate of deposition of cement in and about unfractured perforations under given squeeze-cementing conditions, the proper filtration time to control the amount of deposition to any desired value, and the deposition properties needed in cement slurries to restrict to any desired degree the formation of nodes of cement .Solids inside the casing. INTRODUCTION The deposition of solids against a permeable medium by the process of filtration is an important property of a cement slurry. General recognition of the role of filtration in the use of cement in wells is evident in view of the fact that several patents on low-water-loss cements have been issued during the past few years. In the conventional, high-pressure squeeze-cementing technique, a large volume of cement slurry is usually displaced into the area surrounding the perforated interval after the formation has been fractured hydraulically.&apos; Near the end of the job, the pumping rate is slowed or stopped intermittently in an effort to obtain a high pressure in the wellbore. The way in which a high pressure is obtained is not understood thoroughly. but it is be- lieved to be caused by the deposition of a rigid mass of compacted cement particles either in the fractures of the formations or inside the casing opposite the perforated interval. In a method of squeeze-cementing introduced several years ago, a small amount of cement slurry is squeezed into the perforations at a low pressure to avoid fracturing the formation. The filling of the unfractured perforations with cement particles by the process of filtration is important to the success of this technique. Early in the development of this low-pressure squeeze-cementing technique, laboratory and field-size experiments showed that conventional, neat cement slurries were unsatisfactory if the tubing was extended into or through the perforated section of the casing. The extremely high filtration rate of neat cement slurries caused the deposition of a compacted mass of cement inside the casing and made it impossible to remove excess cement by reverse circulation and difficult to withdraw the tubing. Because the need for cements with a reduced filtration rate was obvioils and urgent, modified cements containing 12 per cent bentonite were used until research was completed on modified cements containing 25 per cent bentonite.< These modified cements were useful in the solution of the immediate problem, but the following questions remained unanswered: (I) what is the optimum filtration rate of cement slurries for this application, (2) how long should the squeeze pressure be applied. and (3) how great are the effects of squeeze pressure and well temperature on the rate of deposition? Furthermore, the relationship of the filtration properties of cement slurries to the dimensions of the perforations and the wellbore was unknown. In order to obtain information relative to these basic considerations, a systematic evaluation of all the factors involved in the deposition of Cement during low-pressure squeeze-cementing operations was initiated. Although the work was directed toward an evaluation of the factors influencing the deposition of Cement in the low-pressure squeeze-

By C. Laird, C. E. Feltner

May different kinds of dislocation structures have been observed in strain-cycled metals and alloys. In order to understand their pattern and causes, an experimental program has been carried out to determine the influence on the dislocation structures of the three variables: 1) slip character of the material, 2) test temperature, and 3) strain amplitude. The results show that at high strain amplitudes cell structures me formed when the slip character is wavy, and that these are progressively replaced by uniform distributions of dislocations as the stacking fault energy is decreased. At lower strains, dislocation debris is formed which consists primarily of dipoles in wavy slip mode materials and multipoles in planar slip mode materials. Temperature merely acts to change the scale of the structure, smaller cells, and clumps of dislocation debris being associated with lower temperatures. It is shown that the results for many metals fit this pattern, which Parallels that occurring in unidirectional deformation. DISLOCATION structures produced by cyclic strain (fatigue) have been examined in a number of metals by transmission electron microscopy. These studies have produced a variety of interesting and often seemingly conflicting results. For example, different investigators have reported such structural features as cells.le4 bands of tangled dislocations,4&apos;5 dense patches or clusters of prismatic dislocation loops, planar arrays,4&apos;10 and various combinations or mixtures of these different structures. Most of these observations have been made on materials which were initially annealed and cyclically strained at low amplitudes resulting in long lives. Recently we have reported observations of the dislocation structures produced in copper and Cu-7.5 pct Al cycled at large amplitudes, resulting in lives of less than 104 cycles.4 These results, examined in combination with those in the literature, have suggested that a common or consistent structural pattern exists. Variations in this pattern appear to be determined chiefly by the three variables, namely, the slip character of the material,4,11 test temperature. and the strain amplitude. To verify this interpretation, we have studied [he influence of the above three variables (in different combinations) on the resultant structures in cyclically strained metals. Copper, fatigued at room temperature, was chosen as a reference state to which all other observations can be compared. The effect of slip character has been investigated by employing fcc metals of different stacking fault energy. Thus aluminum which has a more wavy slip character than copper, and Cu-2.5 pct A1 having a more planar slip char- acter, have been examined. The aluminum samples were fatigued at 210°K thus making their homologous temperature equal to that of copper at room temperature. The influence of temperature has been evaluated by examining the structures in copper at room temperature and 78°K. Finally the effect of strain amplitude was studied by looking at the structures at amplitudes giving lives ranging from 104 to 107 cycles. All of the specimens were examined at the 50 pct life level at which stage the structures have reached a stable configuration.12 I) EXPERIMENTAL PROCEDURE Strip specimens, 0.006 in. in thickness, were prepared from base elements of 99.99 pct purity or greater. Specimens were fatigued by cementing the strips to a lucite substrate which was subjected to reverse plane bending. This method of testing has been described e1sewhere.7 After fatiguing, specimens were thinned and examined in a Philips EM 200 which was equipped with a goniometer stage capable of ±30-deg tilt and 330-deg rotation of the specimen. On the basis of separate calibrations,13 allowances were made for the relative rotation and inversions between the bright-field images and the diffraction patterns. II) RESULTS AND DISCUSSION The life behavior of the materials under different test conditions is shown in Fig. 1 in the form of plots of total strain range vs cycles to failure. Comparisons of structures produced in the different materials were made at amplitudes which produced equal numbers of cycles to failure. The influence of strain amplitude on the structures produced in the reference state material (copper tested at room temperature) is shown in Fig. 2. At the 104 life level the structure produced comprises cells similar to those previously observed.3,4 They are approximately 0.5 p in diam and the cell walls are generally more regular or sharper than those produced by unidirectional deformation.14 At the 10&apos; life level the

Jan 1, 1969

By Frederik P. Agterberg

This paper deals with frequency distributions in the field of mineral resource evaluation when a grid is superimposed on the study area and metallogenetically significant attributes are coded with respect to the cells of the grid. It is shown that the parameters of a negative binomial distribution for frequency of mineral deposits per cell can be derived from the parameters of a gamma distribution for the coded attributes. It is also shown that an exponential model for spatial correlation of cell values and Matheron&apos;s discrete Gaussian model for indirect transfer functions may provide a suitable methodology for relating cell value distribution to cell size.

Jan 1, 1977

Impact Transition Temperatures of Some Pearlite-Free Mild Steels As Affected by Heat Treatments in the Alpha Range H. P. Tardif (Canadian Armament Research and Development Establishment, Quebec)—Mr. Josefsson is to be congratulated for his study of a most difficult subject and for the theories proposed to explain the re- sults. One point which, however, might not have received proper attention is that of the shape of the stress-strain curve at the yield point of quenched and furnace-cooled specimens and of specimens strain aged

Jan 1, 1956

By H. W. Gillett

Unlike most previous Howe lecturers, I had not the good fortune to be associated with Henry Marion Howe, nor to be directly one of his students. Yet, through his writings, he has been my teacher, as he has of all American metallurgists. Instructive as his writings are—I use the present tense because Howe thought so keenly and reasoned so surely, seeing clearly, as if by intuition, what was hazy to lesser minds, that his writings are still vital—it is not those books and papers, nor even the minds he trained in his classes, that were his most outstanding service. It was the spirit of Howe in his approach to the problems of metallurgy, his broad-mindedness and fairness, his recognition of the need for theories and hypotheses to explain metallurgical phenomena, his willingness to use them as servants, as well as his questioning attitude—his refusal to accept them as masters—that comprise his greatest service. This most thoroughly warrants the honor the Institute pays each year to his memory. These traits I so respect and honor in any man that I glory in this opportunity to do reverence to him in whom they were so notably united. Howe&apos;s Discussion of a Creep Problem I have often wished that Howe were still with us to turn his keen insight upon the problems of the use of metals at high temperatures, a field much studied but still very hazy. Indeed, 53 years ago, in a paper1 before this Institute, Howe stated a problem closely allied to some that still perplex metallurgists and engineers dealing with the high-temperature field. Howe was intrigued by a report2 from another old master, Robert Henry Thurston, on the behavior of annealed vs. cold-drawn iron wire, and in order to broaden the foundation for metallurgical generalization, Howe made experiments of his own on copper and silver. In these tests by Thurston and by Howe, the wires were rapidly loaded to determine the

Jan 1, 1939

By J. M. Dahl, R. J. Warrick, O. K. Riegger, H. Van Vlack

A liquid which is rich in oxygen (and silicon) develops at steel rolling temperatures in resulfurized and plain-carbon steels. This liquid fluxes solid manganese sulfide. The composition of the liquid and the resulting microstructures vary with the manganese/silicon/oxygen ratios in the steel. The observations and conclusions zuhich are presented are used 1) to suggest a mechanism for MnS deformation in resulfurized steels, and 2) to rationulize hot-shortness anomalies between plain-carbon and resulfurized steels. 1 HIS is a summary of the dependence of sulfide inclusion microstructures upon steel composition, and an interpretation of the behavior of sulfide inclusions at steel-rolling temperatures. Sulfide inclusions are known to have several metallurgical effects upon steel. Their effects upon hot-shortness are best appreciated. Although hot-shortness is well known, it is questionable whether its mechanism is fully understood because there are several anomalies in our interpretation. For example, why should not high sulfur contents produce extensive hot-shortness in free-machining steels ? A second metallurgical consequence of sulfide inclusions appears because sulfide inclusions improve machinability. Furthermore, globular inclu- sions are to be desired over elongated inclusions. To date, we know that lower silicon contents (< 0.010 pct) favor the globular sulfides, but we do not know why this interrelationship between silicon content and inclusion shape exists. Finally, the evidence is strong that the surface quality of a hot-rolled steel is particularly sensitive to the sulfur content. SUMMARY OF PREVIOUS WORK The role of sulfur in hot-shortness was first suggested during the past century. It is uncertain who was the first to conclude that sulfur was less deleterious in the presence of manganese, and that manganese altered the sulfide phase from a liquid FeS to a solid MnS at steel-rolling temperatures. However, Urban and chipman&apos; emphasized that liquid FeS may accumulate as an interdendritic film during solidification. More recently, Keh and Van lack&apos; showed that the intergranular liquid does not completely surround the metal grains at all rolling temperatures. Rather, a small finite dihedral angle exists when geometric equilibration is attained at

Jan 1, 1962

By Enid C. Plante, K. L. Sutherland

PRACTICAL metallurgists are unanimous in stating that oxidation of mined sulphide ore adversely affects separation of the constituent minerals under standard conditions in a mill. Frequently, the need for different operating conditions in different plants is attributed either to the extent of oxidation of the mineral surfaces or to soluble oxidation products. The investigations reported in this paper study the effect of oxidation on the primary condition necessary for flotation, namely that of adhesion of an air bubble to the mineral. OXIDATION PRODUCTS FROM SULPHIDE MINERALS Weinig and Carpenter1 state that the relative rates of oxidation of some sulphides are: FeAsS > FeS2 > CuFeS2 > ZnS >PbS > Cu2S tetrahedrite. They also show that oxidation is rapid at first, that sulphides of older geological formations are more stable than those of recent date and that mixtures oxidize more rapidly than any one mineral alone. The more rapid oxidation of mixtures is borne out by results of Gottschalk and Buehler2 who found that PbS, ZnS and CuS oxidized 8 to 20 times faster when pyrite was present. Only the end products of oxidation, sulphate and the metal ion, were identified in these tests. Gaudin3 states that pyrite is difficult to oxidize in the laboratory. Winchell,4 using pyrite containing 99.98 pct FeS2, allowed water to percolate through a bed of this ground material. At the end of three months only a trace of Fe +++and S04- were found. Even after 10 months the quantity of Fe+++ was only 7.8 mg and S04- 25.5 mg per liter of percolating solution. Carmichael5 confirmed Winchell&apos;s results on the slow oxidation of pyrite. Usually the oxidation of sulphide surfaces has been conducted in neutral or acid solutions, the acidity being caused by the oxidation products. Eliseev and Nagirnyak6 found that treatment of pure pyrite with lime gave only thiosulphate, but considered it possible that thiosulphate was obtained not by oxidation of the pyrite itself, but by oxidation of calcium disulphide. Mitrofanov7 suggested that thiosulphate was formed by the following process: oxidation of sulphide to give free sulphur (this frequently happens with marcasite), followed by oxidation of the sulphur to sulphur dioxide and reaction of the sulphur dioxide with sulphur to give thiosulphate. Ferric and ferrous hydroxides, or similar compounds, were shown to be present. The Research Staff of the United Verde Copper Co.8 treated ore from the United Verde mine with lime. Thiosulphate, sulphide and polysulphides were stated to be

Jan 1, 1947

By Warnie Flint

PERSONAL INJURY ACCIDENTS According to statistics compiled by the National Safety Council, US Bureau of Mines, American Medical Association, and other agencies, accidental injuries cause more deaths than all the leading diseases. NO one is immune to an accident. Probably the best way to describe an accident is to say that it is an unexpected happening. The automobile driver is not expecting a terrifying crash, the electrician does not expect to be electrocuted, nor is the coal miner expecting the roof to fall on him. All personal injuries will not result in death. There is a multitude of victims who are living proof of what accidents can mean to an individual-victims who are blind, paralytic, missing arms, legs, etc. In most instances the earning power of these individuals is gone, and they are utterly dependent upon family or welfare. For many years there seemed to be an attitude that prevailed in industrial America that accidents were inevitable, and that so many fatalities and injuries should be expected. This, of course, was utter nonsense. Since the birth of such organizations as The National Safety Council, American Society of Safety Engineers, and the US Bureau of Mines, much progress has been made in reducing accidents. The enactment of compensation laws greatly contributed to the progress that has been made. Does this mean that all accidents can be prevented? Unfortunately, it does not. Human psychology indicates that men will work unsafely or perform unsafe acts for the following reasons : 1) Lack of knowledge or skill. 2) Conflicting motivations, such as: (a) to be more comfortable, (b) to save time or effort, (c) to be accepted by a group. 3) Physical or mental condition. Nearly everyone desires his own safety, but not all individuals are willing to do what they know to do to insure their own safety.

Jan 1, 1981

By C. W. Nicolson

THE Tri-State zinc and lead-mining district is in the northeast corner of Oklahoma, the southeast corner of Kansas and the southwest corner of Missouri. The area throughout which active mining has been conducted is about 45 miles long and about 5 miles wide, extending northeasterly from Commerce, Okla., to Alba, Missouri. Although the lead ores were mined on a very small scale in the vicinity of Joplin, Mo., as early as 1848, nothing of any importance was done in the district until 1870, since when both mining and smelting have been prosecuted with considerable vigor. In the beginning the lead ores only were exploited, but within a few years extensive deposits of zinc ores were found and since that time the production of zinc ore has far exceeded that of lead. Both the surface and mineral rights in Missouri and Kansas were under individual ownership by the time ore was discovered. Although some of these rights were purchased by mining companies, most of the mining has been done under leases covering small areas, usually 40 acres, although in the past many leases were given on much smaller tracts. In Oklahoma most of the mineral land had been alloted by the Government to various Indian tribes and although the title to some of these lands had been acquired by various white men before the discovery of the rich Picher field, the title to most of the land has remained with the Indian tribes and the leasing of the mineral rights has been done by the Federal Government for the benefit of the Indians. The Indian allotments were of 200 acres each and some of the mining leases covered entire allotments, although many leases were granted for only 40 acres or even less. Practically all of the leases granted in the past required the erection of a concentrating plant on each lease, a condition that has had a pronounced effect upon the mining and milling methods of the district, since the apparent ore reserves on each tract were too small to justify large

Jan 1, 1938

By Gunnar Almgren

Hole deviation has great consequences on mining economy, especially for long hole drilling technique. First of all the bore hole datas are concerned but also such factors as development, loss of ore and waste rock dilution are influenced. Hole deviation for sublevel open stoping is illustrated with examples from some mines. The deviations are indicated as mean values but also as standard deviation values, owing to their statistical distribution. The economic influence of the hole deviation is especially studied for steep, small lowgrade orebodies, mined with big hole blasting. Hole deviation can thus influence costs up to US$ 3-4 per ton for operating, development, losses of ore and rock waste dilution. This cost is of the same magnitude as the total operating costs for many sublevel stoping mines. The economic savings in accurate drilling are therefore substantial and are worth all attention.

Jan 1, 1981

By Thomas Fraser

UP to the present, there has been no large coal-producing industry in any of the South American countries. Since colonial times, the great mineral and agricultural wealth of that continent has led the people to activities other than the development of manufacturing industries based on coal; and climatic conditions are such that there has been very little demand for solid domestic fuel. However, there are extensive and widely distributed reserves of coal in South America that would make the development of a modern coal industry feasible. That factor is of the utmost significance now, when it is believed that the South American countries are entering the pioneer phase of a broad industrial development. Coal Fields Great areas of coal-bearing formations of Cretaceous and Tertiary ages occur generally throughout the Andean uplift and extend into the coastal range of the Caribbean region far east of Caracas. Thus the west coast countries have adequate reserves of coal, which include a wide range of types and classes. In the eastern part of South America, east of the Cordillera, as in North America, the coal measures are of Carboniferous and Permocarboniferous ages. The principal known deposits in this area are in the southern States of Brazil. Permocarboniferous coals ranging in rank from lignitic to anthracitic are found in the States of Rio Grande do Sul, Santa Catarina, Parana and Sao Paulo. In the great.interior plateau of Brazil, south of the Amazon River, are extensive areas of Carboniferous strata that may contain coal deposits. There are widely scattered reports of findings of coal in&apos; wells and stream beds in northern Piaui and Goias. In the Rio Fresco Valley, explorers have observed outcrops of two beds of anthracite and have brought to Rio de Janeiro samples from these beds. The Fresco is a tributary of the Xingu River that enters the Amazon from the south, but coal could not be shipped by water since the Rio Fresco area is in the upper part of the Xingu Valley, and there is a formidable series of rapids between that area and the lower level of the Amazon River basin. It is doubtful if coal deposits in this general area will be of economic importance for many years to come. Fig. 1 shows the general location of known coal fields of South America that have been explored sufficiently to indicate the presence of workable reserves. The coal deposits of the Andean region are similar in occurrence and general characteristics, as well as in age, to the coals of the Rocky Mountain region of North America. Although the coal fields obviously

Jan 1, 1952

By F. P. Agterberg

It can be useful to model the mean grade values for a metal in mineral deposits containing that metal as representing the extreme value tail of a lognormal frequency distribution for the concentration values of the metal in common rocks of all types. Results for copper and zinc in the Abitibi area of the Canadian Shield are compared to results previously obtained for the Canadian Appalachian region. The lognormal model is also applied to a set of 162 large gold deposits in the Abitibi area. In the second part of the paper, 1311 large and small gold deposits in the Abitibi area are modeled as discrete events. By means of a newly developed spatial clustering model it is possible to predict the variances of random variables for frequencies of deposits in cells of different sizes.

Jan 1, 1981

By R. D. Daniels, T. G. Oakwood

A study was made of the effects of small quantities of hydrogen on the mechanical properties of colum-bium. Tensile specimens, hydrogenated to concentrations of 20 to 200 ppm, were tested at temperatures of 300°, 191°, and 77°K. Although hydrogen was found to have little effect on the strength of columbium, the ductility of Cb-H alloys was found to be quite sensitive to both hydrogen concentration and temperature. At 300°K, an abrupt loss in ductility occurred at a critical hydrogen concentration, although some ductility was observed beyond the tolerance limit. A similar result was found at a lower hydrogen concentration at 191°K. At 77°K, however, a more gradual loss in ductility with increasing hydrogen concentration was observed. Hydrogenated columbium was thus observed to undergo a ductile-brittle-ductile transition. Metallographic examination of fractured specimens revealed extensive porosity at both 77° and300°K which was a distinct function of hydrogen content. At 191°K, although some secondary cracking was noted, the amount of observed porosity was minimal. These observations are interpreted in terms of hydrogen solubility and mobility as a function of temperature and in the role of hydrogen in promoting growth of microcracks. lHE effect of hydrogen on the mechanical properties of the refractory metals is not, at present, completely understood. A number of studies have shown these materials to be susceptible to hydrogen embrittlement. Roberts and Rogers1 have found that vanadium can be embrittled by hydrogen. It was further demonstrated that fracture undergoes a ductile-brittle-ductile transition as the temperature is lowered from 150° to -196°C; i.e., there is a ductility minimum observed at a certain temperature. The ductility is increased by either raising or lowering the temperature from this point. A more complete study by Eustice and Carlson2 on vanadium containing 10 to 800 ppm placed the ductility minimum at about -100°C with variations reportedly due to hydrogen content and strain rate. Ductility minima have also been found at certain temperatures for tantalum containing 7 ppm H3 and 140 ppm H.4 At hydrogen concentrations above 270 ppm, however, the ductility return at low temperatures was considerably reduced.4 In the case of columbium, some disagreement exists in the literature. Eustice and Carlson,5 Wilcox et al.,6 and Imgram et al.4 failed to find a ductility minimum although a composition-dependent ductile-brittle transition was observed. Hydrogen concentrations in these investigations were 20 ppm,5 1 to 30 ppm,6 and 200 to 390 ppm.4 However, Wood and Daniels7 observed a rather pronounced ductility minimum at hydrogen contents ranging from 19 to 252 ppm. Those theories of hydrogen embrittlement involving the precipitation of diatomic hydrogen which have been applies to ferrous metals8-12 do not seem to be applicable to the case of columbium and other exothermic occluders. Such theories propose that extensive crack formation and propagation occurs by the precipitation and expansion of diatomic hydrogen at internal voids and microcracks. However, photomicrographs of hydrogenated columbium do not show any evidence of damage introduced by the sorption and precipitation of diatomic hydrogen; rather, at high hydrogen concentrations, a hydrogen-rich second phase is precipitated.13&apos;14 In addition, a number of these theories require the development of high hydrogen pressures at voids in the structure.8&apos;10&apos;12 This does not appear to be feasible in the concentration ranges discussed in the aforementioned paragraphs. The possible interaction of atomic hydrogen with microcracks resulting from dislocation pile-ups15,16 remains in doubt since pile-ups have not been observed in bcc metals17 including columbium.18 Wood and Daniels7 have put forth the possibility that a hydride precipitation could be responsible for crack nucleation in columbium. Work by Longson19 has shown that hydrogen embrittlement of columbium parallels the bulk solubility limit; i.e., as the solubility increases, for instance with temperature, the amount of hydrogen necessary to cause embrittlement also increases. Although a hydride precipitation appears attractive as a means of nucleating microcracks in columbium, what require more intensive study are the low-temperature anomalies which have been observed, i.e., the ductile-brittle-d&apos;ictile transition characteristics. Also, the hydrogen concentrations where embrittlement occurs are often below the bulk solubility limits determined by Albrecht et al.13,14 and Walter and Chandler.20 This work is an attempt to determine more definitively the effects of concentration and temperature on the mechanical properties of dilute Cb-H alloys. EXPERIMENTAL PROCEDURE Ultrahigh-purity columbium rods, obtained from the Wah Chang Corp., were cold-reduced by rotary swaging. A chemical analysis is given in Table I. The material was cut into cylindrical blanks 1.50 ±0.005 in. long. Individual specimens were either given a stress relief anneal at 750°C or recrystal-lized at 1200°C. Resulting microstructures were either a "bamboo" structure characteristic of a wrought material or a recrystallized structure with a grain diameter of approximately 100 n. All heat treatments were carried out in a vacuum of 10-5 Torr or less.

Jan 1, 1969

By G. S. Cole, H. Biloni, G. F. Bolling

An experimental investigation of sovlze low .melting point alloys sJtows that a substvucture of isolated depressions can be the first manvestation of constitutional supercooling on solid-liquid interjaces veuealed by decanting. Electron-tni cvop vobe and wletallo gvaplic esanzinations, in tlze bulk belzind the interjace, oj the segregation associated with these isolated areas substantiate tlzei&apos;v depressed nature, since a solute of ko < 1 is enriched, and a solute of ko > 1 depleted. In contrast, the pox structuve, a set of projections often veported in the literature, leaves no trace oj. segvegation. These obserl;atims, accovlrpanied by a brief review of recent literature, point to inconsistencies between experirrental obsevvation and the idea that the fornzation of a projection is a causal step in the development of a cellular substructure. An argument is presented to show instead how it is plausible for substantial depvessiom to form in the pvesence of constitutional supercooling at dislocations threading the solid-liquid interjace. THE development of constitutional supercooling during growth from the melt leads to the formation of the cellular solidification substructure. This well-founded association between structure and instability has been basic in understanding cellular substructure and micro segregation; however, the initial formation of structure seems unclear. Rutter and Chalmers,&apos; in definitive experiments and theory, noted that in the presence of constitutional a planar interface might break down: "resulting in the formation of a small projection on an initially plane or uniformly curved interface." That is, the breakdown from a planar to a cellular interface was implied to be initiated via a projection into the unstable liquid. Later, Walton et (11. found that a structure of isolated projections, termed "pox", appeared at solid-liquid interfaces decanted under growth conditions near the onset of constitutional supercooling; the pox were taken as the indication of the instability promoted by the supercooling. Tiller and Rutter4 in their extensive work studied the shape transitions at decanted interfaces which were generally observed to proceed as— pox, "irregular cells", elongated cells, regular (hexagonal) cells, and so forth. The pox varied in size from lo-&apos; to 1CT4 cm, and tended to disappear as cells increased in number and regularity, but as noted,4 the first real array of cells did not seem to be a development from the pox. In fact these authors implied a lack of connection because they stated that the pox are denser on "irregular cells", and as cell boundaries increase in number (i.e., the cells become smaller) there is less need for the pox which do dis- appear. Thereafter, most authors dealing with either experiment or theory have accepted the reality of pox and have used them as a criterion for the onset of constitutional supercooling. In contrast, Spittle, Hunt, and smiths have now suggested that pox are irrelevant artifacts comprised of such things as entrapped oxide. This proposal invokes the observations of weinberg6 and chadwick7 each of whom have shown that the act of decanting leaves a residual liquid on a decanted interface; the remnant solid layer of the order 10 p may thus contain particles that might have been transported from the external surfaces, or elsewhere, during decanting. With the incentive of this suggestion,= some further experiments and a reexamination of the literature have been conducted, in order to question the validity of pox as evidence of an instability and to examine the initial development of the cellular substructure. 1) EXPERIMENTS Single crystals of zone-refined tin (-99.9999 pct) were grown from the melt in a controlled fashion with various, small concentration additions of lead and antimony, for which ko < 1 and > 1, respectively. The crystals were decanted at conditions near the onset of constitutional supercooling and were thus appropriate for observation of slight perturbations. It was possible to observe two types of small departure from smooth or "planar" interfaces in both cases of lead or antimony additions. Some were projections and others, if in regular array of any type, were depressions. The crystals were etched with suitable reagents progressively dissolving the decanted interface surface; projections left no record, but depressions were continuously associated with spotlike areas contrasting with the rest of the interface. Traverses were made with the beam of an electron microprobe across the regions of contrast; with lead addition the persistent spots were lead-rich, and with antimony addition the persistent spots were antimony-poor. This is consistent only with a dominant role for depressions, because if the projections had left spots but were incorrectly catalogued, a reversed observation should have been made; that is, the Pb(ko < 1) should have been depleted and the Sb(ko > 1) enriched. In the work of Cole and inegard, and elewhere, regular arrays of structure associated with the initial stage of instability have been shown, in photographs and represented as pox or projections. We believe this to be erroneous, by inference, since whenever a regular array was observed, in the present examination, it consisted of depressions, regardless of the nature of the solute, ko 1. Fig. 1 is reproduced8 as an ideal example of the possible optical illusion involved; the observer can satisfy himself from the distribution of illuminated areas that the markings are depressions. Fig. 2 from the present investigation is an interference photograph of an interface similar to that in Fig.

Jan 1, 1967

By C. D. Williams, C. E. Ells

The susceptibility of quenched and aged Zr-2.5 wt pct Nb alloy to embritt2ement during irradiation has been examined for a number of solution temperatures and aging times. Material quenched from temperatures approximately 40°C below the transus has high tensile ductility, and this ductility is insensitive to aging at 500°C or to irradiation. If, however, the material is quenched from temperatures above the transus it becomes highly susceptible to loss of ductility either from aging at 500 or from irradiation. Inter granular failure is characteristic of the materials having low ductility. The distribution of the equilibrium phase is found to control the susceptibility to embrittlement by restricting 6 grain growth during heat treatment and thus influencing crack propagation. IN zirconium, as in titanium, -stabilizing alloy additions are used to obtain high strengths via quench and age heat treatments, and the Zr-2.5 pct Nb alloy has been developed1 because of its strength advantage over the Zircaloys. Early in the development of the Zr-2.5 pct Nb alloy the problem of 13 embrittlement was appreciated, and for this reason the solution temperature was chosen below the p transus.&apos; In the course of irradiation studies on quenched and aged Zr-2.5 wt pct Nb alloy it was found&apos; that irradiation introduced an important aspect of p embrittlement, riz., material quenched from the phase and aged 24 hr at 500°C was severely embrittled by moderate doses of neutron irradiation. This effect had not been studied in titanium alloys. In titanium the metallurgical features leading to 0 ernbrittlement were found to be structures with: a) coarse a platelets at the grain bondaries, b) finely dispersed a uniformly distributed throughout the (0) matrix,6 c) Widmanstatten a-13 with more than 50 pct P, d) the presence of some metastable p transformation products,3 and e) large prior -phase grain size.5 Alternatively, the presence of a uniform distribution of coarse a was conducive to high ductility and a structure largely of equiaxed a was very dctile. The detailed mechanisms of the embrittlement have not been worked out for all of these conditions, although weakness at either a-matrix boundaries or prior p grain boundaries have been prominent in the eculation. It was proposed that acicular a might act as a mild notch, and low ductility has been associated with easy fracture along its boundary.&apos; There have been two opposing suggestions for the source of the high ductility associated with equiaxed a phase. JaffeeB proposed that this a would accept a large por- tion of the oxygen, thus increasing the ductility of the matrix, whereas after study of a Zr-Nb-Cu alloy Weinstein and oltz proposed that the a phase, softer than the martensitic matrix, acted to blunt cracks formed in the matrix. In the present work we have studied the effect of neutron irradiation on the ductility, particularly the P embrittlement, of the Zr-2.5 wt pct Nb alloy. By a variation of solution temperature and aging time a variety of metallurgical conditions have been examined, and a range of resultant ductilities obtained. The ductility has been related to the material microstructure and mode of fracture. EXPERIMENTAL The alloy used in the present work came from two separate ingots fabricated into rod of 3/8 or i in. diam, Table I. For both batches the P transus temperature was approximately 890° C. Most of the heat treatments were done directly on lengths of the j} in. diam rod, after which the tensile test specimens were machined. Quenching was achieved by dropping rods from a dynamic vacuum into water, the cooling rate estimated to be 2 100°C per sec. For aging the rods were encapsulated in evacuated silica tubes. Round tensile test specimens, with gage diam and length 0.160 and 1.0 in., respectively, were used throughout and pulled at room temperature or 300°C on Instron tensile machines, at a crosshead speed of 0.05 ipm. Specimens were irradiated in the NRX and NRU reactors, in facilities described in previous publications.&apos;0 The metallurgical conditions examined have been: All tensile test specimens were machined with axes in the axial direction of the swaged rod. Although the specimen had a degree of preferred crystallo-graphic orientation with basal plane normals both parallel with and perpendicular to the tensile axis, the material was comparatively isotropic." The techniques of thin foil examination in the electron micro-

Jan 1, 1970

By H. l. Burghoff, A. I. Blank

The state of knowledge bearing on the stability of copper under stress at elevated temperatures is generally known to be in need of revision and extension. The present investigation, dealing with the creep characteristics of a deoxidized copper of low residual phosphorus content, is intended to contribute in some small measure toward this end. The experimental data presented herein have been correlated by methods of evaluation and interpretation familiar to those who are concerned with crecp of metals. In practice it is common, if not requisite, to use structurally stable materials at elevated temperatures. It is frequently desirable, however, to test materials under conditions that produce structural change, in order to determine the extent of such change and its effect on physical properties, thus making it possible to establish accurately the limiting conditions to which such materials may be safely exposed. The creep characteristics of the drawn copper wire of this investigation arc directly associated with its structural instability at elevated temperatures. Complete realization of this fact is essential to the evaluation of its creep resistance under various conditions. Creep results should apply to steady deformation under equilibrium conditions, but these are seldom attained in only one or two thousand hours. It will be shown that steady creep rate for copper at useful stresses does not usually begin until considerably more time has elapsed. A wholly satisfactory substitute or shortcut for extensive creep testing does not appear to be evident in the application of mathematical analyses to limited experimental data. Material A single lot of phosphorized copper wire was drawn down to 0.125-i11. diameter with a final reduction of 84 per cent. After mechanical straightening, a portion of this wire was annealed to an average grain size of 0.013 mm. in a controlled-atmosphere furnace. The composition and initial properties of the copper in these two conditions are listed in Table I. Photomicrographs of the original structure are shown in Fig. I.

Jan 1, 1945