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By A. Wahab Khair

"Geologic materials emit transient noises when stressed /1/. The rate and pattern of these transient noises or acoustic emissions (A.E. hereafter) depend on the stages of deformation of the material /2/. It has been demonstrated that rock/coal fracture processes under stress consist of three distinctive stages--crack initiation, propagation and ultimate fracture--and that coalescence of numerous cracks leads to ultimate failure rather than the propagation of a single crack /2,3/. This paper presents an analysis of fracture formation in rock/coal specimens subjected to straight wedge indentors using A.E. technique.The effect of specimen geometry, wedge indentor angle, confining pressure, and material anisotropy on fracture type (tension, extension, and shear crack), fracture length, and fracture intensity were studied. Two types of material mainly Berea sandstone and Coal Berg No. 2 coal were used in this study. Prior to the experiment the mechanical properties of both sandstone and coal were determined using rectangular specimen (Figures 1 a) in standard compression tests and are given in Table 1. In this study cylindrical and rectangular specimens were first prepared to proper dimensions of 2 in. x 1.5 in. and 3 in. x 1.5 in. x 1.5 in. (5.08 cm x 3.81 cm and 7.62 cm x 3.81 cm x 3.81 cm), respectively and then instrumented with SR-4 strain gages as shown in Figure 1. The instrumented specimens were then tested under four distinct load boundary conditions as illustrated in Figure 2. During a typical experiment the instrumented specimen was placed in a specially designed loading jig (Figure 3) where a predetermined lateral pressure was applied mechanically to the specimen by adjusting the inner plate of the confining chamber via screw while monitoring strains in the specimen. Using rock/coal elastic constants and measured strains, a predeter¬mined lateral pressure was applied to the specimen. Then a vertical load was applied by the straight edge of a wedge indentor attached to the upper platen of the universal loading machine via ball and socket arrangement (Figure 4). The arrangement allowed uniform application of load in a straight line manner on the surface of the specimen. During the test a number of parameters namely strains, load and A.E. rates were recorded (Figures 5a-b)."

Jun 1, 1988

By D. Malovichko

Seismic events and pillar failures observed in two platinum mines in the Rustenburg area, South Africa, were investigated. We studied the sources of approximately 300 largest seismic events recorded in 2009. Moment tensors of these events were estimated from amplitudes and polarities of P- and S-waves. The inverted mechanisms contain isotropic implosive components in many instances. Analyses of uncertainty of the moment tensor solutions confirmed the significance of the implosive component in general. Several documented cases of pillar failure were considered in detail. For each of these a seismic moment tensor was calculated from an elastic stress model assuming an instant removal of a failed pillar. The geometries and magnitudes of the theoretical seismic moment tensors are in agreement with the observed (i.e. inverted from seismic data). The results indicate that either pillar failure or fracturing in the proximity of the reef (within a fraction of the dominant wavelength of seismic waves) are responsible for a significant portion of the large events recorded in these mines.

Jan 1, 2012

By Shengli Wu, Jiacong Zhang, Kai Gu, Bingjie Wen, Heng Zhou

In practical production process, the average of silicon content in hot metal (HM) of COREX process (the average is 1.58%) is obviously higher than that in blast furnace (the value is below 0.6%), which leads to an increase in the cost of steelmaking. In this work, the factors affecting and impact mechanism of silicon content in HM were investigated by statistical analysis using actual operating data. The analysis indicates that the fuel rate, binary basicity of slag and the temperature of HM are positively correlated with the silicon content, while the sulfur content of HM and binary basicity of burden are negatively correlated with the silicon content. On this basis, a back propagation neural network was developed to predict and control the silicon content in HM. All the findings of this work are useful for guiding and optimizing the COREX operation.

Mar 1, 2018

By W. G. Sinclair

The North Texas district incorporated in this paper corresponds with the Railroad Commission's District No. 9, and includes the counties of Archer, Baylor, Clay, Cooke, Foard, Hardeman, Jack, Knox, Montague, Wichita, Wilbarger, and Young.† Table I,Oil and Gas Production in North Texas District, has been changed to conform with the nomenclature of pools designated by the Commission in order to facilitate compilation of the data, since most of the companies operating in the area are coming more and more to recognize one central authority in the matter of naming each new oil pool. No effort is being made to discuss the structural characteristics of the region, since it is generally known by oil men that most of the oil and gas comes from Pennsyl-vanian, with some of less importance from the Mississippian and Ordovician. Development during 1944 There were 1550 wells drilled during 1944, an increase of 450. Of this number, 677 were completed as oil wells, and 11 as gassers. Production increased 1,505,025 bbl., making the year's total 43,172,005 bbl. of oil having an average gravity of 40". Development generally, however, was somewhat disappointing. The 47 new pools, extensions, or new pay horizons in old fields, had a combined initial production of only 19,146 bbl. It is estimated that these wells added approximately 10,000,000 bbl. to the reserves. The largest single addition to the reserves was in the Caddo conglomerate in the Hildreth pool, Montague County. During the year, 66 wells were completed as the result of three extensions, I to 136 miles west, northwest and north of the field. Young, Archer, and Clay were the most active counties. Eleven new potential - oil fields were developed in Young County, nine in Archer and nine in Clay. Outlook for 1945 In spite of the fact that exploration as a whole was disappointing in 1944, prospects for increased development are bright for 1945. At the close of last year, 2.1 geophysical crews were operating in the district, which, together with the Ohio Oil Company's No. I W. R. Ross, a wildcat Strawn discovery in King County, 1 1/2 miles beyond the west boundary of district 9, stimulated a lease play extending over four counties. Two of them, viz., Foard and Knox, are in the area incorporated in this report. Acknowledgments The writer is indebted to Mr. C. W. Hanley, Zone Agent of the North Texas District, and Mr. William M. Lourcey, head of the Land, Leasing and Scouting Department for the Gulf Oil Corporation, both of Fort Worth, Texas, for permission to prepare this paper.

Jan 1, 1945

By P. J. Soltis

Direct as well as indirect evidence of a-phase ordering was found in a "near-a" type titanium alloy, Ti-8Al-1Mo-1V. The annealed alloy showed an anomalous decrease in second-stage creep rate at 950°F (510°C) and 47,500 psi. Anomalous increases were noted in initial yield stress after 500 hr creep exposure and in tensile strength after 1100 hr creep exposure. Debye-Scherrer X-ray diffraction patterns obtained on fine-grained polycrystalline speci-ment showed much line broadening and development of superlattice lines after 500 hr at 510° C. Examination with the light and electron microscopes failed to reveal phase changes in thermally exposed material, but detailed metallography is presented illustrating the plastic and fracture characteristics of the alloy. Electron-metallographic evidence is presented, however, which shows the nature of the nucleation and growth of ordered regions from the disordered a in annealed material. In the original phase diagram of the binary Ti-Al system constructed by Ogden et al.1 aluminum was shown to be soluble in a titanium over a wide temperature range at concentrations up to about 30 pct. Subsequently, a number of papers2-7 have appeared which indicate the existence of either intermetallic compounds and/or ordered phases in the a field up to 25 pct Al. In the most recent of these, Goldak and Gordon paw7 have determined unequivocally the ordered hexagonal D019 structure for Ti3Al in a 25 pct Al alloy. No superlattice lines were observed above 1112°F (600°C). Previously, the embrittle-ment encountered by Crossley and Carew4 in low- temperature heat treatments of binary Ti-Al alloys low in aluminum had been attributed to the appearance of a new phase in light micrographs. In the present work, direct as well as indirect evidence is presented showing the existence of a-phase ordering in what is essentially the binary Ti-8A1 alloy containing small percentages of the ß stabilizers molybdenum and vanadium, i.e., the "near-a" Ti-8Al-1Mo-1V alloy. Although Bohanek and Kessler8 have shown that this alloy has good stability at temperatures up to 1100°F (593°C), the present work shows instability at 950°F (510°C) where long exposure times were used. Light and electron microscopy proved very useful in revealing the mechanical behavior of ordered a and led to the conviction that ordered "near-a" alloys may have remarkably good properties and useful engineering applications.

Jan 1, 1965

By James K. Stanley

Preferred orientation, particularly in irons and low-carbon steel, is a phenomenon that is both of considerable importance and theoretical interest. At times it is a liability and at other times an asset. In deep-drawing operations, preferred orientation is extremely undesirable because it necessitates trimming operations and increases scrap loss. Furthermore, oriented metals are likely to crack more easily than randomly oriented material because the forming of symmetrical and unsymmetrical shapes out of preferentially oriented metals and alloys increases the probability of rupture in regions of high stress, owing to differential ductility.' In the electrical industry, on the other hand, preferentially oriented silicon irons are in demand for transformer application because of the improved magnetic permeabilities in the rolling direction.2 This phenomenon of preferred orientation in soft magnetic materials has been responsible for the tremendous improvement in transformer design and construction in recent years. Directional properties in metals have received a great deal of attention in the metallurnical -literature,3-9 in which much of the information reported about orientation has been obtained by conventional methods, mechanicai properties and X-rays. A wealth of data has been obtained and often at a great expenditure of time. The recent introduction of the magnetic torque measurements on ferromagnetic materials provides a very simple and rapid method of evaluating orientation. The judicious use of the method can supply important information, but it should be borne in mind that such studies must be supplemented by X-rays, optical methods,10 and etch and pressure figures" to get a rational understanding of the orientation phenomena. No claims are made that the magnetic torque of evaluating orientation will reveal the behavior of the metal in deep drawing. For this purpose the accepted tests for deep-drawing quality must be used. For a good drawing stock, which must have low impurities, desirable grain size, ductility, strength, hardness, good surface, random orientation, and good recrystallization behavior, it cannot be expected that any simple test will be satisfactory for appraising all the factors. The only factor on which the magnetic method can be used is orientation, which is, of course, of considerable importance. When directionality can cause a 10 to 15 per cent change in tensile strength and a IOO to 300 per cent change in tear length,12 it goes without saying that a reliable as well as rapid method for detecting these changes would be desirable. There are certain inherent advantages in testing orientation by the torque method: The method is rapid with the proper type of equipment; no elaborate preparation of specimens is required—it is only necessary to punch or machine a I-in. disk of the sheet material and insert it into the testing device.

Jan 1, 1944

By Thomas Fraser, H. F. Yancey

Prior to the war just ended, Germany was the greatest coal producer in continental Europe. In 1943 the production of coal, bituminous and higher in rank, together with brown coal calculated to the equivalent amount of bituminous coal, is estimated to have been about 240 million metric tons, according to the War Department. Before the war production in Germany exceeded consumption. No other country in continental Europe except Poland had a large surplus. However, England's surplus was the largest in Europe as a whole. Before World War II the Ruhr Basin normally supplied about 70 pet of the total production of high-rank coal, the Saar and Aachen about 6 pet each, Upper Silesia about 14 pet, and Silesia and Saxony the remainder. Nearly one third of the brown coal was produced in the Rhineland, a little less than one half in central Germany nest of the Elbe River, and about one fourth east of the Elbe. Bituminous coal and brown coal together constituted by far the most important energy resources of the old German Reich. Bituminous coal furnished nearly 70 pet of the total energy requirement, brown coal supplied about 25 pet, and water power, wood, petroleum and alcohol together aggregated only 7 pet. Because it was the most important single mineral resource of Germany, an excess of coal enabled the Reich to import nearly all the other mineral products that she lacked, such as iron ore from Lorraine. The area adjacent to the coal fields was supplied with gas from an interconnected grid. Similar electric grids are based on brown coal with the power stations at the mines. Coal tar provided the foundation for the development of the extensive German chemical industries as exemplified by the I. G. Farbenindustrie. For almost a century, German scientists have been adequately supported both by the State and by industry in studying improved methods of utilizing coal. In Germany the mineral rights were reserved by the State and ordered eatraction of coal was enforced. Each lease comprised a relatively extensive area. which accounts for the generally large size of the mines and mining companies In 1938 there were 160 mines in the Ruhr, with a total output of 125 million tons but 90 pet of the production was controlled by 20 companies. By far the largest single coal-mining company in Germany was the Gelsen-kirchener Bergwerke A. G., which produced nearly 27 million tons in the Ruhr in 1937. Second was Saargruben A. G. a State-owned company operating in the Saar, which produced 'lore than '3 million tons. Third was Bergwerksgesellschaft Hibernia A. G., with 10 million tons, also in the Ruhr. Briquettes are made from both bitumillous coal and brown coal, but in 1938 some 44 million toils of brown-coal bri-

Jan 1, 1947

By Thomas Fraser, H. F. Yancey

Prior to the war just ended, Germany was the greatest coal producer in continental Europe. In 1943 the production of coal, bituminous and higher in rank, together with brown coal calculated to the equivalent amount of bituminous coal, is estimated to have been about 240 million metric tons, according to the War Department. Before the war production in Germany exceeded consumption. No other country in continental Europe except Poland had a large surplus. However, England's surplus was the largest in Europe as a whole. Before World War II the Ruhr Basin normally supplied about 70 pet of the total production of high-rank coal, the Saar and Aachen about 6 pet each, Upper Silesia about 14 pet, and Silesia and Saxony the remainder. Nearly one third of the brown coal was produced in the Rhineland, a little less than one half in central Germany nest of the Elbe River, and about one fourth east of the Elbe. Bituminous coal and brown coal together constituted by far the most important energy resources of the old German Reich. Bituminous coal furnished nearly 70 pet of the total energy requirement, brown coal supplied about 25 pet, and water power, wood, petroleum and alcohol together aggregated only 7 pet. Because it was the most important single mineral resource of Germany, an excess of coal enabled the Reich to import nearly all the other mineral products that she lacked, such as iron ore from Lorraine. The area adjacent to the coal fields was supplied with gas from an interconnected grid. Similar electric grids are based on brown coal with the power stations at the mines. Coal tar provided the foundation for the development of the extensive German chemical industries as exemplified by the I. G. Farbenindustrie. For almost a century, German scientists have been adequately supported both by the State and by industry in studying improved methods of utilizing coal. In Germany the mineral rights were reserved by the State and ordered eatraction of coal was enforced. Each lease comprised a relatively extensive area. which accounts for the generally large size of the mines and mining companies In 1938 there were 160 mines in the Ruhr, with a total output of 125 million tons but 90 pet of the production was controlled by 20 companies. By far the largest single coal-mining company in Germany was the Gelsen-kirchener Bergwerke A. G., which produced nearly 27 million tons in the Ruhr in 1937. Second was Saargruben A. G. a State-owned company operating in the Saar, which produced 'lore than '3 million tons. Third was Bergwerksgesellschaft Hibernia A. G., with 10 million tons, also in the Ruhr. Briquettes are made from both bitumillous coal and brown coal, but in 1938 some 44 million toils of brown-coal bri-

Jan 1, 1947

By James K. Stanley

Preferred orientation, particularly in irons and low-carbon steel, is a phenomenon that is both of considerable importance and theoretical interest. At times it is a liability and at other times an asset. In deep-drawing operations, preferred orientation is extremely undesirable because it necessitates trimming operations and increases scrap loss. Furthermore, oriented metals are likely to crack more easily than randomly oriented material because the forming of symmetrical and unsymmetrical shapes out of preferentially oriented metals and alloys increases the probability of rupture in regions of high stress, owing to differential ductility.' In the electrical industry, on the other hand, preferentially oriented silicon irons are in demand for transformer application because of the improved magnetic permeabilities in the rolling direction.2 This phenomenon of preferred orientation in soft magnetic materials has been responsible for the tremendous improvement in transformer design and construction in recent years. Directional properties in metals have received a great deal of attention in the metallurnical -literature,3-9 in which much of the information reported about orientation has been obtained by conventional methods, mechanicai properties and X-rays. A wealth of data has been obtained and often at a great expenditure of time. The recent introduction of the magnetic torque measurements on ferromagnetic materials provides a very simple and rapid method of evaluating orientation. The judicious use of the method can supply important information, but it should be borne in mind that such studies must be supplemented by X-rays, optical methods,10 and etch and pressure figures" to get a rational understanding of the orientation phenomena. No claims are made that the magnetic torque of evaluating orientation will reveal the behavior of the metal in deep drawing. For this purpose the accepted tests for deep-drawing quality must be used. For a good drawing stock, which must have low impurities, desirable grain size, ductility, strength, hardness, good surface, random orientation, and good recrystallization behavior, it cannot be expected that any simple test will be satisfactory for appraising all the factors. The only factor on which the magnetic method can be used is orientation, which is, of course, of considerable importance. When directionality can cause a 10 to 15 per cent change in tensile strength and a IOO to 300 per cent change in tear length,12 it goes without saying that a reliable as well as rapid method for detecting these changes would be desirable. There are certain inherent advantages in testing orientation by the torque method: The method is rapid with the proper type of equipment; no elaborate preparation of specimens is required—it is only necessary to punch or machine a I-in. disk of the sheet material and insert it into the testing device.

Jan 1, 1944

By Z. Pilecki

This work concerns the identification of weak zones in the structure of a rock mass endangered by outburst of gases and rocks in the Rudna copper ore mine at greater depths (approximately 1200 m). A special methodology has been undertaken for the recognition of that threat in the wake of an outburst in the mine in 2009. No similar phenomena have been previously recorded in KGHM Polska Miedz copper ore mines. The research described in this paper was carried out in the new part of the deposit prepared for mining. Geophysical methods were used: seismic tomography and borehole ground penetrating radar (BGPR), along with particular identifications using geological engineering methods. In the researched area, Permian layers of sandstone and shale clay (Weissliegendes formation) and of Zechstein dolomite (top of Rotliegend formation) and anhydrite occur in the copper ore deposit. The rock layers are characterized by variable thickness and intensity of mineralization, varying internal structure, and local fracturing containing different gases and water. It is assumed that accumulation of gases occurs in the tectonically fractured dolomite. The study was focused on the recognition of the structure and properties of the dolomite layer lying directly within the roof of excavations. The first tests were performed with seismic tomography for the recognition of anomalous changes in the elastic properties of the rock mass. The results of these studies were used to design a control borehole for a detailed geological engineering assessment and BGPR surveys with 100MHz antennas. Seismic tomography enabled the identification of changes in Pwave and S-wave velocity, the Vp/Vs ratio, dynamic Poisson's ratio and dynamic Young's modulus. It was clear that seismic anomalies required verification by other methods. The BGPR survey was performed in a specially designed borehole, passing through the selected seismic anomalies. While the borehole was being drilled, the outflow of gases was identified, with varying amounts of CH4, CO2, and H2S detected, as well as water outflow. The results of BGPR confirmed the location of a reservoir of water and gases, about 30 m in length, found in layer of dolomite. The direct cause of the BGPR anomaly was assumed to be intensive fracturing, a greater content of clay material in the dolomite, and the presence of water in the fractured zone. The BGPR image was correlated with information on lithology, fracturing based on the RQD index and additional information acquired during drilling about water and gases surveys and other symptoms. The achieved results also showed a very strong correlation between the location of the zone containing gases and water and the anomalous S-wave velocity and field of dynamic Poisson?s ratio, and to a lesser extent other seismic parameters. It was found that the other measured seismic anomalies may be of the same nature as those identified in the control borehole and accordingly will require the implementation of detailed identification. The performed tests have also shown the usefulness of geophysical methods to identify geodynamic hazards under the geological and mining conditions of the copper ore deposit in the Rudna mine.

Aug 1, 2013

By K. R. Brown, P. L. Krawchuk

In-situ recovery (ISR) is under increased investigation as a viable methodology for the extraction of minerals in ore bodies that may be uneconomic to mine by traditional methods or for resources situated in locations where underground and surface mining operations are not feasible. Although the concept of ISR is relatively new with respect to hard rock applications, it is not a new technology; it has been used successfully in potash and uranium mining and also in heavy oil extraction for years where it has been proven to be both technically and commercially viable. ISR allows for the extraction of metals and minerals without the need to mine large amounts of ore that need to be processed at surface. The ore stays in-situ and only the valuable metals and minerals are produced to surface in a process that produces very little to no waste rock or tailings. This paper aims to discuss the geological conditions that make ISR amenable to an ore body as well as the application of maturing technologies such as advanced directional drilling and the creation of artificial permeability that will help to access deep ore bodies and enhance or create favorable recovery conditions for ISR in the ore body. INTRODUCTION In-situ recovery (ISR), also referred to as in-situ leaching, is a potentially disruptive technology for the mining industry. ISR is under increased investigation as a viable methodology for the extraction of valuable minerals that may be uneconomic to mine by traditional methods or for deposits situated in locations where underground and surface mining operations are not feasible. Although the concept of ISR is relatively new with respect to hard rock applications, it is not a new technology; it has been used successfully in potash mining, uranium mining and also in heavy oil extraction for years where it has been proven to be both technically and commercially viable. Recently there has been increased interest in deploying ISR in hard rock applications due to a number of factors: the drive for environmental stewardship is stronger than ever, technological advances in drilling, blasting, and leaching are strengthening ISR economics, and a large inventory of ore bodies exists that are not feasible to mine or extract using conventional open pit or underground mining techniques. ISR allows for the extraction of valuable metals and minerals without the need to mine large amounts of ore that need to be processed at surface. The ore stays in-situ and only the valuable metals and minerals are produced to surface in solution via a recovery process that produces very little to no waste rock or tailings. Where the right conditions exist, the ISR process has a much smaller environmental footprint (Hiam-Galvez, 2018) and potentially much lower capital and operating costs than using conventional mining techniques.

Jan 1, 2019

By Peter Zhang, Mark Van Dyke, Ted Klemetti, Morgan Sears

Room-and-pillar mining is a mining method used in the United States to extract coal from underground, and pillar recovery is widely practiced for maximizing coal recovery and mining economics. Under certain conditions, room-and-pillar mining can create high stresses in coal pillars resulting in a coal outburst. These outbursts represent one of the more severe safety hazards in underground coal mines, potentially causing injuries and fatalities. Over the past ten years, coal outbursts have resulted in three fatalities in U.S. room-and-pillar mines. Though coal outbursts generally occur under deep cover, they are more likely to occur during pillar recovery and under multiple-seam mining conditions. Coal outbursts are generally associated with strong roof and floor and heavy loading of coal pillars, but it is difficult to predict whether, where, and when they will occur. In this respect, risk management provides a proactive tool to prevent coal outbursts in room-and-pillar mining by identifying mining areas with high risk of outburst and mitigating the risk accordingly.

Apr 26, 2022

By H. I. Aaronson

Isothermally formed plates of proeutectoid a, lengthen at approximately the rates predicted by the Zener-Hillert equation, indicating that their lengthening kinetics are controlled by the volume diffusion of chromium in the ß matrix. Solution annealing treatments in the vicinity of the transus introduce a second mode of transformation, in which the lengthening rate is at least 1.8 x 104 faster than predicted by this equation. Little or no volume diffusion appears to accompany the latter transformation. The Presence of oxygen is evidently a Prerequisite for the occurrence of this reaction. X HE effects of thermal history prior to the initiation of transformations which proceed by nucleation and diffusional growth are currently evoking considerable interest. The rate of nucleation (but not the rates of growth) of pearlitel and of bainite,2 and the over-all rates of aging reactions in Al-cu3 and Al-si4 alloys have been shown to be appreciably dependent upon thermal history in the solid-solution region"' or in the two-phase region prior to the onset of pre~ipitation.3,4 In none of these reactions, however, was the transformation mechanism changed by variations in the temperature-time path used to reach the reaction temperature. Preliminary experiments reported by M. K. McQuillan5,8 and a systematic investigation by Farrar and Margolin7 have disclosed that the transformation behavior of hypoeutectoid Ti-Cr alloys is considerably more sensitive to thermal history. Qualitative evidence strongly suggests that not only the rate of nucleation but also the rate of growth and even the mechanism of the ß — a reaction can undergo remarkable changes when a solution annealing treatment in the vicinity of the ß/a +ß, or transus temperature, is interposed between a high-temperature solution anneal (conventionallq at 1000°C) and the isothermal reaction treatment. The present investigation was undertaken in an attempt to ascertain the nature and origin of these effects. Study of the changes in the kinetics and morphology of the ß - a, reaction produced by varialtions in thermal history was the primary means employed for this purpose. EXPERIMENTAL PROCEDURE The compositions of the alloys used in this in~esti~ation are given in Table I. These alloys were homogenized for 5 days at 1050° C in evacuated (2 x 10 -5 mm of Hg), zirconium-gettered fused quartz capsules. The capsules themselves were enclosed in a porcelain chamber evacuated with a mechanical pump during the homogenization anneals. Upon completion of homogenization, the alloys were cooled to room temperature and then reheated to 550°C for 3 1/2 days in order to transform the alloys to a finely divided mixture of a and TiCr2, and thus provide an approximately constant initial mi-crostructure. Individual specimens were sealed in evacuated and internally gettered Vycor capsules and heat treated as previously described.8,9 EXPERIMENTAL RESULTS Ti-10.64 Pet Cr. This investigation was largely performed on the 0.64 pet Cr alloy. The "base"

Jan 1, 1962

By D. W. Levinson, L. F. Mondolfo, N. A. Gjostein

MANY investigations are reported in the literature on the age hardening of Al-Mg-Zn alloys but most of them are concerned mainly with mechanical property changes. The present investigation was started to determine the structural changes in an AlMgZn alloy. The alloy composition was chosen in the existing phase diagram" so as to lie on the quasi-binary section Al-(AlZn)Mg Actually, it was found that the diagram as published was inexact at the lower temperatures and that the phase in equilibrium with aluminum at the lower temperatures is not the ternary compound. Technique The alloy used for the investigation was prepared from high purity materials and the resulting composition as determined by chemical and spectro-graphic analysis was: Zn, 6.17 pct; Mg, 2.13 pct; CU, 0.03 pct; Si, 0.009 pct; Fe, 0.005 pct; and the remainder, aluminum. An ingot -in. thick was cast, homogenized, hot and cold-rolled to strip 0.064-in. thick for dilato-metric and powder work, and to foil 0.005-in. thick for single crystal work. Solution treatment temperature for all specimens was 475°±5°C for periods of at least 1 hr, either in air furnaces or lead baths. Aging was done in oil or Pb-Bi baths controlled to within ±3°C. The aging was investigated at the following temperatures: room (30°), 130°, ZOO0, 260°, and 300°C. For the dilatometric study, the length changes were measured continuously, at temperature, using strips of alloy 10 in. long, shaped as channels to eliminate undesirable deflection due to bending. To compensate for thermal expansion and contraction due to the variations in the temperature of the aging baths, the dilatometers were built of the same alloy as the one being tested, with the same shape and size, but with material fully annealed. Gages on which 0.0005 in. could be read and 0.0001 in. estimated were used to measure the dilation. Length changes were also measured at room temperature. Strips approximately 10 in. long were solution-treated, quenched, and measured in a supermicrome-ter in which 0.0001 in. could be read and 0.00001 in. estimated. The specimens were immediately aged for a given time, remeasured, and then the cycle was repeated, including the solution treatment. The error of measurement with this technique was somewhat larger, but the results confirmed those obtained by continuous measurements. The sheet used for the dilatometric work was checked to determine grain orientation. Both X-rays and etching methods revealed a rather coarse grain size but only a negligible amount of preferred orientation. Thus, volume changes calculated from length changes are not invalidated by preferential orientation effects. Pieces of the sheet used for the dilatometric work were also used for the metal -lographic work. Filings for the powder X-ray study were produced from a homogenized piece of sheet. These filings were magnetically purged of iron, screened to 200 mesh, sealed in a Pyrex tube containing an argon atmosphere, and solution-treated. When quenching, the glass tube was broken, so that the powder dropped directly into cold water. After drying with alcohol, the powder was sealed into capillary tubes containing an argon atmosphere and then aged for the required times. In spite of all these precautions the three strongest lines of a( Al2o) appeared in all patterns, and were used as internal standards. By the use of these standards, accurate corrections for film shrinkage were obtained. For the back reflection patterns, annealed nickel powder was mixed with the specimen to act as internal standard. A preliminary investigation was made in small (57.3 mm diam) powder cameras. From these patterns the changes which took place in the solid-

Jan 1, 1957

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

THERE has been considerable discussion among A metallurgists and others interested in the development of titanium alloys as to the nature of the fine line markings which appear in the microstruc-tures of unalloyed titanium and a titanium alloys. These markings have been variously called x phase, etching pits, and twins. Figs. 1 to 3 show typical examples of the line markings as they appear, respectively, in high purity iodide titanium, commercial purity titanium rod, and a high purity a alloy containing 0.2 pct N. The commercial purity titanium sample, shown in Fig. 2, contains both line markings and some spheroidal retained-ß phase. The ß phase seen in this micrograph should not be confused with the line marking, since it originates from the iron present as an impurity in the sponge metal. It will be noted that the line markings seem to have a definite orientation pattern with respect to the grains and in titanium noticeably resemble the precipitation occurring in artificially aged high purity Al-Cu alloys. This similarity led to the hypothesis that the line markings observed in titanium and a titanium alloys resulted from precipitation of some unknown phase. With the work of Hägg1 and McQuillan2 as background, there was little reason to suspect hydrogen of being responsible for the line markings. Hagg reported that up to 33 atomic pct H was soluble in a titanium, and McQuillan reported an a solubility of up to 8 atomic pct. Furthermore, McQuillan examined metallographically a 5.1 atomic pct H alloy quenched from 300°C and stated that the structure appeared to be a single-phase a solid solution. Line markings have been observed frequently and were first noted by Jaffee and Campbell3 in 1949. They did not observe them in vacuum-annealed titanium and a Ti-O and Ti-N alloys, but did observe them in Ti-H alloys containing 0.25, 0.5, and 1 atomic pct H. They stated that it was doubtful that the markings were a second phase based on hydrogen, because 1 atomic pct was far from the accepted solid solubility of hydrogen in titanium. Finlay, Resketo, and Vordahl,4 in 1950, concluded that the markings were a true second phase as a result of observations on their etching characteristics. Anderson5 Commenting on these markings in titanium was inclined to associate them with hydrogen, but was loath to call them titanium hydride, because of the reported high solubility of hydrogen. Work at Battelle Memorial Institute for the Navy Bureau of Aeronautics," done concurrently with the work described in this paper, provided information on the experiment converse to that described by Jaffee and Campbell in 1949. This work showed that the amount of line markings in unalloyed titanium could be decreased by vacuum annealing at elevated temperature. It was suggested that this was the result of removal of hydrogen; previously, the data of Jaffee and Campbell9 howed that the markings appeared when hydrogen was added. Recent work at Battelle for the Ordnance Corps, Department of the Army, which is described here, now establishes the identity of the markings as a titanium hydride phase. A sample of high-purity titanium rod 1/4 in. diam, 0.009±0.001 wt pct H (0.43 atomic pct), Fig. 1, was resistance heated in a 0.05 micron vacuum for 41/2 hr at 1500°C. During the early states of heating, the pressure increased to 150 microns, indicating that gases were being evolved. After cooling in vacuum, the iodide titanium rod was analyzed for hydrogen. Vacuum-fusion analysis showed 0.0006 ±0.0003 wt pct H (0.03 atomic pct) to be present.* Metallographic examination of the vacuum-annealed rod showed only a transformed ß structure. There was no evidence of fine line markings, Fig. 4. A section of this vacuum-annealed rod was cold rolled to 0.040 in. thick sheet and annealed for 1 hr

Jan 1, 1953

By Peter N. Holtham, Mary M. Ng

"Resistivity measurements of minerals in the laboratory are commonly made with a low DC voltage source. Common test voltages specified in the ASTM Standard D257 are 100, 250, 500, 1000, 2500, 5000, 10000 and 15000 V, however 100 and 500 V are the most frequently used. Resistivity results obtained in the laboratory have been used to infer the electrical behaviour of minerals undergoing electrostatic separation. However because the voltages employed in electrostatic separation in the plant are of the order of thousands of volts, typically greater than 15000 V, whether the laboratory results are applicable as a predictor of plant performance is a critical question. It is unclear whether resistivity values taken at a low voltage are characteristic of those seen in electrostatic separation, in which the minerals are exposed to a much higher voltage. No definitive answer could be found in the literature.In this work, the resistivities of zircon, rutile and ilmenite were measured in a corona field for the first time. The measurement principle was based on a technique developed to measure fly ash resistivity in electrostatic precipitators, however the test apparatus and findings are novel.Resistivities of rutile and zircon were found to be easy to measure. The values measured in a corona field were several orders of magnitude less than those obtained with a dc voltage of 100 V. Evidence of back corona was observed with zircon. When the voltage drop was greater than the sample layer could withstand a localised electrical stress developed, resulting in a voltage breakdown, at which point a sudden surge of corona current (back corona) was detected in the sample layer. Rutile, on the other hand, exposed to the same conditions as that of zircon (i.e. same temperature and applied voltage) did not exhibit any sign of back corona. Its resistivity across the range of test voltages (14 to 33 kV) remained fairly constant."

Jan 1, 2003

By Shiro Ban-ya, John Chipman

The effects of many alloying eletnents on the acticity coefficient of sulfur in liquid iron have-been studied by the equilibriutn in the reaction Sfin Fe) + Hz = HzS at 1550°C'. Results are expressed in terms of a concentration variable for a nonmetallic or for a substitutional metallic solute. Activity coefficient of sulfur, defined as increased by B, Al, C, Si, Ge, Sn, P, As, Sb, Mo, W, Co, and PI. It is decreased by Cu,Au, Ti. Zr, V, h'b, Ta, Cr, ,23n, and Ni. Irulues oj. the interaction coejficient 0i = 6 In are labulated. The same interactions are expressed also in terms of atom fraction and of weight percent. The thermodynamic properties of sulfur in liquid iron have been fairly well established. Our recent paper1 reported new determinations of activity coefficient up an atom fraction of 0.12 and equations based on a careful review of all published data. The effects of alloying elements on the activity of sulfur have been studied by several investigators,2"11 especially by Morris and Williams for silicon,' by Morris and Buehl for carbon,~ and by Sherman and Chipman for manganese. phosphorus, and al~minum.~ However, the effects of some important alloying elements remain to be determined. The purpose of this investigation was to determine the effects of many alloying elements on the activity of sulfur in Fe-S-j ternary systems. EXPERIMENTAL METHOD This study was based on experimental determination of equilibrium in the reaction at 1550°C: The same apparatus and procedure as described in our previous paper have been retained, and the same corrections were applied for dissociation of H2S. The alumina crucibles used in the experiments consisted of four separate compartments. In a given experimental run. kach of three alumina crucibles held four different samples of about 3 g each which reached equilibrium in the same gas atmosphere and temperature. The charges were made up of electrolytic iron, pure iron sulfide, and desired alloying elements, which were pure metal or master alloys made in the laboratory. The weighed samples were held for 4 to 12 hr in the prepared atmosphere at 1550°C. They were then low- ered to be cooled as quickly as possible. The quenched metal beads were crushed to avoid the errors of segregation in the ingot. The sulfur content was determined gravimetrically and alloy content by appropriate chemical analysis. CALCULATIONS The apparent equilibrium constants of Eq. [I] are expressed as follows from the corrected gas ratios and sulfur concentrations: The term K" is the observed equilibrium constant in any given ternary solution, K' is the value for the Fe-S binary solution. and the limiting value of K' in the infinitely dilute solution is designated by K, which is the true equilibrium constant in Eq. [I]. In the thermodynamic treatment of nonmetallic elements in a metallic solution, it has been suggested1' that the lattice ratio has certain advantages over other variables to express the concentration of solute. In interstitial solid solutions the lattice ratio zj is proportional to the ratio of filled interstitial sites to those which remain unfilled. The equations derived for the activity of the solute using zj as the concentration variable are found also to be applicable to liquid solutions containing nonmetallic solutes when the nonmetal is treated as if it were interstitial. For this purpose we adopt the following definitions: The quantity vj which is negative for interstitial solutes is taken as -1 for nonmetallic and +1 for metallic solutes. For purposes of calculation however ; j may be assigned a value which results in a linear relation such as shown in Figs. 1 to 15. The activity coefficient of sulfur, Qs, and equilibrium constant. K(z). are defined as follows: According to a Taylor series expansion. the logarithm of the activity coefficient of sulfur in Fe-S-j ternary system is: However, the value of 6 In */6zi remains constant through a broad range of dilute solutions and the terms of higher order are negligibly small. As a consequence, Eq. [6] is simplified as follows:

Jan 1, 1970

By D. Kunstelj, M. Stubicar, A. Tonejc, A. Bonefacic

A. Bonefafcic, D. Kunsfeli, M. Stubicar, and A. Tonejc The present communication is concerned with the variation of the texture in aluminum wires with die angle and temperature, at constant speed of extrusion. Experiments were carried out concurrently on refined samples, with a stated purity of 99.997 pct pure A1 and commercial samples of 99.5 pct Al. Ingots of refined aluminum samples were machined to 30-mm-diam by 150-mm-long billets. These billets were transformed to 5-mm-diam wires by drawing. The final form, suitable for examination, was obtained by extrusion through conical-face dies with a 1-mm hole diam and extrusion ratio 5:l in diam. The initial form of the commercial aluminum samples was drawn wire 5 mm in diam. These samples showed a poorly defined texture with (111) as a major and (001) as a minor component. A similar defined texture appeared in the refined aluminum samples after drawing to 5 mm diam. Conical-face dies with different angles (defined by the axis and the generating line of the cone) were used in our experiments. The values of the angles were 27, 35, 45, 57, 63, and 90 deg. The extrusion container was fitted with a heating element and controller permitting temperatures up to 600°C to be maintained within i5"C. Extrusion was performed at 250°, 300°, 350°, 400°, and 500°C at constant speed (approximately 1 mm per sec) and constant die reduction. The extrusion product was a wire 1 mm in diam and approximately 20 cm long. In order to remove the surface layer with the "conical" texture and to reduce the absorption by the X-ray examination of the samples, the extruded wire was etched to 0.22 mm in diam. Experiments were performed in the middle sections of the 20-cm-long wires. In addition to the die of l-mm hole diam, dies with a 1.5-, 0.7-, 0.6-, 0.5-, and 0.4-mm hole diam and 63-deg die angle were constructed. In our experiments we did not find in these ranges any important difference concerning the texture of the extruded wires and we continued our work solely on the 1.0-mm die. The diffracted X-rays (Cu K radiation) were recorded photographically. Diffracted intensities were measured on the (111) reflection with a microphotometer. The relative amounts of texture components were determined from the areas under the diffracted maxima. We found the texture of extruded aluminum wires to be strongly influenced not only by the temperature of extrusion and the purity of the sample but also by the form of the die. It is generally admitted that cold-drawn aluminum wires have mainly a (111) texture with a small amount of (001) component, Table I of Ref. 1. In our experiments with wires extruded in conditions represented by Fig. 1, in some cases a single (001) texture was obtained. If these wires were drawn repeatedly at room temperature, X-ray measurements revealed a duplex (001)-(111) fiber texture. Further drawings increased the (111) and decreased the (001) texture component. In Fig. 1 the percentage of material oriented with (001) parallel to the extrusion direction is represented as a function of the temperature and the die angle (a), for commercial and refined aluminum samples, respectively. From these diagrams we may draw the following conclusions. The slope of the die (a) influenced more strongly the texture at the lower rather than the higher temperatures. Again, a stronger influence was found in the case of the commercial in comparison with refined aluminum samples. In the case of the commercial aluminum samples the amount of material with (001) texture increases with increasing wire temperature in an approximately linear manner. This effect is less pronounced in the pure aluminum samples, with the exception of the die with a = 45 deg. In this case the (001) texture decreases with increasing temperature, as shown in Fig. 1. Component (001) is more pronounced in higher-purity aluminum samples. Our experiments led to the conclusion that both (001) and (111) components are essentially stable in extruded aluminum wires. As we obtained a single (001) texture starting with a sample of drawn wire in which the (001) component was very weak, our experiments revealed that the (001) component is not a remnant of the initial texture; this is in disagreement with the findings of Vandermeer and McHargue.1 We gratefully acknowledge discussions with Professor M. Paic. 1 R. A. Vandermeer and C. J. McHargue: Trans. 7MS-AME, 1964, vol. 230, p. 667.

Jan 1, 1969

By Klaus Schwerdtfeger

The equilibria in the Cr-N system have been investigated in the temperature range 1100° to 1310°C by reacting chromium powder with Nz-Hz gas mixtures. The solubility of nitrogen in chromium in equilibrium with chromium subsitvide ("Cr,N") is given by Chromium subnitride is nonstoichiotnetric; its nitrogen content is always less than that corresponding to the formula CrzN. The lattice paranzeters of quenched samples have been measured; c, and a. parameters are found to increase with increasing nitrogen content. The growth rate of the subnitride layer on chromium plates was measured by a thermogravimetric technique, using a silica spring balance. The self-diffu-sivity obtained from the theoretical analysis of the parabolic rate constant is found to decrease with increasing nitrogen content, i.e., with decreasing vacancy concentration in the nitrogen sublattice. The intrinsic nitrogen diffuivity is derived from another series of rate measurements using "CrzN" plates; the intrinsic diffusivity, DN = 3.2 X 10-a cmZ sec-' at 1200 C, is found to be essentially independent of- the subnitride composition. The concentration gradient was measured in a chromium subnitride layer by the X-ray method and found to be consistent with the derived diffusivity value. TWO chromium nitrides are known to exist:' the nonstoichiometric subnitride "CrzN" and the nitride CrN. In the present work the kinetics of the formation of chromium subnitride from chromium and nitrogen have been investigated at 1100" and 1200°C. In additional experiments the relevant equilibria have been measured. The data are used to evaluate the diffusivity of nitrogen in chromium subnitride. Since chromium nitrides are often found in chromium-containing steels, the results are expected to be helpful in the interpretation of the chemical reactions between chromium steels and nitrogen. Equilibria in the Cr-N system have been determined by several investigators.2"3 The rate of nitriding of chromium was measured by Arkharov et a1 .' in ammonia in the temperature range 800" to 1200°C. The parabolic rate law was observed. Due to the undefined nitrogen activity of the ammonia atmosphere, it is dif- ficult to interpret these rate data theoretically. An additional difficulty arises from the fact that the two-layer scale consisting of CrN and "Cr2N" was formed at the temperatures below 1030°C. The rate of nitriding of technical chromium (95 pct) was measured by Zaks in nitrogen at -1 atm in the temperature range 800" to 1300°C. EXPERIMENTAL METHODS The chromium samples were reacted with Nz-HZ gas mixtures in a vertical tube furnace, wound with Pt-10 pct Rh resistance wire. The gas-tight reaction tube was of high-purity recrystallized alumina. In nitrogen solubility measurements the nitrogen content of chromium was determined by the Kjeldahl method, on samples quenched in the cold part of the furnace. The nonstoichiometry of the subnitride and the nitriding rates were measured thermogravimetrically using a sensitive (+0.1 mg) silica spring balance. For the equilibrium measurements samples of 1 g of chromium powder contained in high-purity alumina crucibles were used. In order to remove most of the oxygen and nitrogen impurities from the chromium, the samples were initially annealed in purified hydrogen until a constant weight was obtained. The chromium plates (approximate dimensions 2 by 1 by 0.08 cm) used for the rate measurements were machined from ingots obtained by arc-melting of iodine-processed chromium. According to manufacturers' specifications the purity of the chromium powder was 99.9 pct Cr and that of the iodine-processed chromium 99.99 pct Cr. Our own spectroscopic analysis of the chromium powder yielded 0.02 pct Fe, 0.05 pct Mn, 0.05 pct Si, and 0.02 pct Ti as major impurities with all the other detectable elements below 0.005 pct. The nitrogen partial pressure of the gas phase was controlled by mixing prepurified hydrogen and nitrogen with constant pressure head capillary flowmeters. Oxygen and water vapor were removed from the mixed gas by passing it through columns of platinized asbestos (450°C) and anhydrone. The gas flowed upward in the furnace with flow rates of 300 to 500 cu cm per min (25"~). Gas tightness of the furnace system was ensured by pressure checks at regular intervals. The furnace temperature was controlled electronically in the usual manner. The reported temperatures were measured with a Pt/Pt-10 pct Rh thermocouple and are estimated to be accurate within ±$C The X-ray measurements were made with a Debye-Scherrer camera and a diffractometer using chromium radiation {\Ka = 2.29092A). EQUILIBRIUM MEASUREMENTS The experimental results of the equilibrium measurements are contained in Tables I to In. Fig. 1 shows the solubility of nitrogen in solid chromium in the temperature range 1100" to 1310°C. In Figs.

Jan 1, 1968

By P Craig, A Crosky, H Ramandi, S Saydam, H Chen

Frequency of reports on premature failure of rock bolts and cable bolts have increased in past two decades. Such a failure threatens both the safety of underground mine workers and the economic viability of the operations. Herein, we report on analysis of rock bolts and cable bolts failed recently in three underground mines in Australia. Magnetic particle inspection (MPI) and scanning electron microscope (SEM) techniques were used to study the failed bolts. MPI showed a number of subcritical cracks on the surface of the bolts. The majority of the cracks in both cable bolts and rock bolts were initiated from the base of ribs (indentation) where the stress concentration was high. SEM examinations showed tearing topography surface (TTS) in all failed rock bolts and cable bolts. These indicated that the failure occurred through hydrogen assisted stress corrosion cracking (HISCC). The results of this study enhanced the understanding about the failure of rock bolts and cable bolts in underground mines. CITATION:Chen, H, Ramandi, H, Craig, P, Crosky, A and Saydam, S, 2018. Analysis of premature failure of rock bolts and cable bolts failed in underground coal mines, in Proceedings The Fourth Australasian Ground Control in Mining Conference (AusRock), pp 407–413 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 30, 2018