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By G. R. Love, C. C. Koch

The changes in superconducting properties with aging time have been studied ,for the pecipitation reaction in a Tc-30 at. pct V alloy. Superconducting critical temperature, upper critical field, and relative critical current density were determined by ac susceptibility techniques. Aging produces changes in critical temperature of both matrix and precipitate which can be rationalized by compositional effects. maximum flux pinning (critical current density) occurs at a time during aging when subgrain boundaries are completely decorated with precipitates and the subgrain centers remain precipitate -free. The particular effectiveness as barriers to flux motion of planar defects which enclose regions of low deject density is discussed. THE precipitation of a second phase can dramatically modify the superconducting properties of type I1 super-conductors. According to Livingston and Schadler1 one might expect changes in the primary, secondary, and tertiary superconducting properties of the material. Changes in matrix chemistry caused by precipitation can alter the fundamental superconducting parameters; critical temperature, Tc, and thermody-namic critical field, Hc. The concimitant changes in electron mean free path (reflected in normal state resistivity) can affect the critical fields Hc 1, IIc2, Hc3. Finally, the presence of precipitate particles may hinder the motion of flux lines and may considerably improve the current-carrying capacity in high-field superconductors. The influence of precipitation on superconducting properties has been studied in a number of systems.2 Magnetization measurements have been used to study the influence of precipitates on flux pinning in lead-base alloys by Livingston3 and Evetts et al4 In these alloys precipitates induced magnetic hysteresis and flux trapping. The amount of hysteresis increased with the volume fraction of precipitate and decreased with coarsening of the precipitate. Jn an Al-Zn alloy5 and an A1-Ag alloy6 the initial precipitate size was presumably smaller than a coherence length and coarsening increased magnetic hysteresis5 and critical current density.6 The influence of precipitation on superconducting properties has also been studied in several of the commercially interesting Ti-Nb7-10 and zr-Nb11 alloys. The maximum in critical current density for these alloys was confined to a narrow range of either isothermal aging time" or isochronal aging temperature7 during the precipitation reaction. Thus, experimental evidence and theoretical considerations suggest there is an optimum precipitate size, spacing, and density, and a critical composition with respect to the matrix for flux pinning. What these "optimum" values might be and the relative importance of each is still not clear, although a few generalizations can be made. It is generally accepted1' that particle sizes smaller than the coherence length or larger than the inter-flux line spacing are poor pinning centers. In high Hc2 materials, precipitate sizes for maximum values of critical current density lie in the range of 50 to 2000Å,9,7 and there are indications that increasing dissimilarity between precipitate and matrix produces increasing pinning force.13 Because of several interesting features of the aging reaction in a Tc-30 pct V alloy, we have chosen to study the influence of precipitation on the superconducting properties of this alloy. The physical metallurgy14 and a survey of the superconducting properties" of the Tc-V alloy system have been reported. The Tc-V phase diagram is presented in Fig. 1. At 1500°C the Tc-30 pct V alloy is in the single phase 6 field. Samples quenched from the 6-phase field have a CsCl structure X-ray diffraction pattern at room temperature and it has been proposed that the 6 structure is closely related to the bcc lattice.14 When held isothermally below the eutectoid temperature, 115O°C, the 6 phase decomposes into the CsCl and hcp phases.

Jan 1, 1970

By G. R. Leverant, C. P. Sullivan

Re crystallized TD-nickel mi-2Th0,) in both coated und uncoated conditions was fatigued at 1800°F at total strain ranges varying .from 0.2 to 0.75 pct. The fatigue life of uncoated inaferal, Nf, was related to the total strain range, ?eT, by (2Nf/021AeT = 0.014. A duplex Al-Cr pack coating increased the fatigue life by about a factor of two. The cracks that led to failure in both coated and uncoated material were initiated at the outer surface, indicating that the mechanical properties of the surface layers were important in determining fatigue life. Crack propagation and subsurface crack initiation in the TD-nickel occurred preferentially at grain boundaries with cavitation at thoria particle-matrix interfaces an integral part of the grain boundary fracture process. The importance of both the grain morphology developed during thermome chanical processing of TD-nickel and the distribution of thoria particle sizes to fatigue resistance are discussed. THE fatigue properties of only a few dispersion-strengthened metals have been studied at temperatures 0.5 Tm;1,2 among these have been lead and aluminum containing oxide dispersions. TD-nickel is a material of interest for application in aircraft gas turbine engines, but little fundamental information is available on its behavior under cyclic loading conditions. In this study, the low-cycle fatigue properties of TD-nickel were determined at 1800°F with emphasis on the 101-lowing; 1) the relation of the grain morphology produced during thermomechanical processing to crack initiation and propagation; 2) the role of thoria parti-cles in the fracture process; and 3) the effect of an oxidation resistant coating on fatigue life. I) MATERIAL AND EXPERIMENTAL PROCEDURE The TD-nickel was supplied by DuPont as a 5/8-in. thick plate which had been subjected to a proprietary series of thermomechanical treatments with a final anneal at 2000°F for 1 hr in hydrogen. The composition of the material is given in Table I. At the test temperature of 1800°F, the 0.2 pct offset yield stress was 15,000 psi, and the elongation and reduction in area were 4.6 and 3.0 pct, respectively. The microstructure of this material has been previously described.&apos; Briefly, it consists of an array of lath-shaped grains, about 0.15 mm in thickness, with the long dimension of each grain parallel to the primary working direction, Fig. 1(a). The presence of very small annealing twirls, Fig. l(b ), together with the absence of extensive dislocation networks, Fig. L/C), indicated that the material was in the recrystal- Table I. Composition of TD-Nickel ThO2 2.3 vol pct C 0.0073 wt pct lex 0.01 wt pct Cr 0.01 wt pct Cu 0.004 wt pct S 0.001 wt pct Ti <0.001 wt pct Co <0.01 wt pct Ni bal lized condition. Commercial TD-nickel sheet has a similar grain size and shape, but unlike the present material is not recrystallized as evidenced by the absence of annealing twins and the presence of a well-developed dislocation substructure.4 The plate material had Young&apos;s moduli in the rolling direction of 22 x 106 psi and 13 x 106 psi at room temperature and 1800°F, respectively, indicating a texture with a strong {100}<001> component in agreement with previous observations on recrystallized TD-nickel sheet.596 The 2.3 vol pct of thoria particles were uniformly distributed although some clustering and stringering of larger particles was occasionally seen. The average diameter of the particles was 450 and the calculated mean planar center-to-center spacing was 2100Å. Two specimens were coated with a duplex A1-Cr pack coating. The coating was somewhat nonuniform from one position to another along the gage length. An area of the coating after testing is shown in Fig. 2. Electron microprobe analysis revealed the following zones in the various lettered regions indicated in Fig. 2: A) a bcc matrix of B-NiA1 with some chromium in solid solution along with a fine dispersion of a chromium-rich second phase which was probably precipitated during cooling from the test temperature to room temperature; B) fcc y&apos;-Ni,Al with some chromium in solid solution; C) porosity; D) a two-phase mixture of a chromium-rich solid solution containing nickel and aluminum and a small volume fraction of a nickel-rich solid solution having approximately the same composition as the immediately adjacent portion of region E, E) the TD-nickel substrate containing chromium in solid solution to a depth of 5 to 10 mils. As expected from the nature of the diffusion processes involved,7 the thoria particles were present only up to the layer of porosity, region C, Fig. 2. The measured thickness of the coating proper, zones A to D, after testing was 1 to 2 mils. The specimen design and testing techniques have been previously discussed.&apos; Stressing was axial and parallel to the lath-shaped grains (i.e., parallel to the rolling direction). The total strain range was controlled between zero and a maximum tensile strain varying from 0.2 to 0.75 pct. (The test at 0.2 pct total strain range was switched to load control at 1030 cycles at which point the peak tensile and compres-

Jan 1, 1970

By N. S. Bornstein, M. A. DeCrescente

ThE nickel and cobalt base superalloys employed in gas turbine engines under some conditions&apos; oxidize at an accelerated rate when exposed at elevated temperatures to atmospheres containing minor quantities of sea salt. It is generally agreed by investigators in the field that the major steps comprising this phenomena of accelerated oxidation, also called hot corrosion or more commonly, sulfidation, are a) a slag composed primarily of Na2S04 is formed on turbine components, b) the protective oxide scale is rendered ineffectual, c) the slag reacts with. the substrate to form metal sulfides, and d) the substrate is rapidly oxidized. Sodium sulfate, a minor constituent of sea salt, is formed within the gas turbine engine from the reactions between NaC1, the major constituent of sea salt, and the oxides of sulfur.&apos; Depending upon concentration, engine compression ratio, and temperature, the Na2S04 will be present in the gaseous or condensed state. It has been determined that in order for sulfi-dation to occur the Na2S04 must be present in the condensed state.&apos; Although a number of sulfidation mechanisms have been postulated, there is no consistent explanation of oxide scale breakdown and subsequent catastrophic oxidation. Some investigators believe that after oxide scale breakdown, the Na2SO4 reacts with the substrate to form lower-valent sulfur compounds. The accelerated rate of oxidation is due to oxidation of a nickel-sulfide phase." Other investigators believe that sulfur from the fused salt reacts with chromium in the alloy to form chromium-rich sulfides; thereby depleting the alloy of an element which imparts oxidation resistance.3,4 This publication will demonstrate that the accelerated rate of oxidation associated with sul-fidation is due to interactions between Na20, a con-stituent of NazSO.,, ancl the substrate. The aim of this study was to separate and determine the effect of compounds of sulfur and sodium on the oxidation kinetics of various nickel-base superalloys, in order to elucidate the sulfidation mechanism. The work reported herein is sponsored in part by the Naval Ship and Development Center-Investigation of EXPERIMENTAL PROCEDURE The nickel base alloys B-1900, U-700, and Waspaloy were chosen for this study. The nominal compositions are presented in Table I. The specimens, approximately 1 in. by 1 in. by 0.060 in. received in the "as cast" condition were polished with 600 grit emery, washed, and rinsed with acetone immediately prior to oxidation experiments. Sulfida-tion attack was duplicated in the laboratory by apply-ing a saturated aqueous solution of Na2S04 onto the al loy substrate and subsequently exposing the specimens in oxygen at elevated temperature. The method of Na2S04 application is described elsewhere in detail.6 In another set of experiments the affected substrate microstructure associated with sulfidation was reproduced free of the normal oxide scale, by reacting and diffusing elemental sulfur into the alloy. The experimental procedure is also described elsewhere in detail. All oxidation studies were performed using an Ainsworth thermobalance type RV-AU-1, which is readable to 0.01 mg and is reproducible to ±0.03 mg. The specimens, introduced into a heated furnace, were exposed in the temperature range 800" to 1000°C

Jan 1, 1970

By Tibor Stefansky, John E. Dorn

MOTT and Nabarro1-5 were first to illustrate the importance of the flexibility of dislocations in accounting for the strengthening that metals undergo due to the presence of internal-strain centers. Such strain-centers might arise from a number of causes such as radiation damage, the presence of semicoherent and coherent precipitates and clusters, as well as individually dispersed interstitial and misfit substitutional solute atoms. Each strain-center induces positive and negative shear stress fields on the slip planes of the surrounding alloy matrix. In order to effect plastic deformation, therefore, the alloy must be subjected to sufficiently high applied shear stresses to push dislocations past all such internal stress fields. If dislocations were inflexible and moved as rigid lines, they would be equally pushed and pulled by internal stress fields. At this extreme the strengthening would be vanishingly small. Dislocations, however, are not rigid; they are flexible and extensible. They wiggle between positive and negative strain-centers, thus increasing their line energy at the expense of their interaction energy with strain-centers. cottrel16 and Friedel7,8 have independently presented lucid reviews of the significance of the Mott-Nabarro dislocation-flexibility concept to the strain-center strengthening of alloys. Their analyses however were only semi-quantitative. There is evidence in the recent literature of renewed interest in a more rigorous analysis of flexibility. Thus, Gleiter9 and Gerald" have shown that the calculated strain-energy interaction between a dislocation and the stress fields of coherent precipitates can be seriously in error if the flexibility of the dislocation is not taken into account. This report will be concerned with a more detailed analysis of the problem based on the following approximations: 1) Although many types of strain-centers exist, the following analysis will be limited to the case of solute-atom strain-centers in fcc substitutional alloys. 2) To facilitate the analysis by avoiding statistical considerations, the strain-Centers are assumed to be in regular arrays on the slip plane. Although the quantitative results are somewhat dependent on the type of array that is assumed, the qualitative trends are similar for various arrays that were studied. 3) An adjustment of the results from those for square arrays to those for the more realistic case of a random distribution of strain-centers is accomplished by adopting the interesting statistical theory first introduced by Kochs,11,12 elaborated on by Dorn, Guyot, and stefansky,13 and analyzed by Foreman and Makin14 in their computerized experiments. 4) For simplicity the dislocation lines are taken to wiggle about their edge orientation and no correction is applied to their line energy for deviations from edge configurations or for the elastic interaction between segments of the now curved dislocation. It will be shown that for extremely low concentrations of atomic strain-centers the strengthening increases with the square root of their concentration. For slightly higher concentrations the strengthening rate becomes less rapid. At a critical concentration a maximum strength is obtained and a decrease in the strengthening takes place as the concentration of solute atoms is further increased. These trends are a direct consequence of dislocation flexibility. They arise from changes in the amplitude of the waviness of the dislocation line at the yield stress with solute atom concentration. Despite the simplifying assumptions that were made, the results agree qualitatively with appropriate experimental data. I) STRESS FIELDS ON SLIP PLANES Internal stresses are introduced in a lattice whenever a host atom of radius ro is replaced by another that has a different atomic radius. According to the classical theory of linear elasticity,15 the stress field about a solute atom at the origin of a spherical coordinate system is given by arr=-4G€(?_0)3 ffflfl ="W =2G€{t) f°rr^ro(l+e) UJ where G is the shear modulus of elasticity and Y, = ro(l + E) is the radius in situ, of the substituted atom. As shown by ~shelb~,&apos;~ this approximation assumes that the bulk modulus of elasticity of the substituted atom is identical with that of the host species. ~abarro&apos;~ suggested that the strain E can be deduced

Jan 1, 1970

By F. H. Froes, D. H. Warrington

Electron microscope evidence which indicates that TaC may precipitate at random sites in the matrix is presented. Initially the particles are almost spherical and coherent with the matrix. However, as they grow in conditions in which there are insufficient vacancies to relieve lattice strain, the particles rapidly lose coherency in two directions and continue to grow as plates with approximately the full lattice mismatch strain present perpendicular to the plane of the plate. The necessary relief of strain comes from dislocations loops which do not become visible until the later stages of aging. The rapid decrease of apparent strain to low values of appoximately 1 pct at small particle sizes arises not from a complete incoherency but from applying a model wrong for the particle shape and strain distribution. PREVIOUS work has shown that MC-type carbides may precipitate intragranularly in austenitic stainless steel on dislocations,1&apos;2 in association with stacking faults,3&apos;4 and randomly through the matrix,5-7 In investigations of the matrix precipitate by thin-foil electron microscopy, considerable lattice strain has been found to occur around the precipitating phase.7&apos;8 Attempts have been made to evaluate the amount of lattice strain by using the methods developed by Ashby and brown.9,10 Values of the linear strain, much less than the 17 pct theoretical mismatch (for TaC), have been reported; it has been suggested that this is due to either a loss of coherency1&apos; or vacancy absorption which occurs during either the initial nucleation or growth of the precipitate." This report is an extension of earlier work7 that dealt with the precipitation of TaC from an 18Cr/12Ni/ 2Ta/O.lC alloy after it had been quenched from 1300°C and aged between 600" and 840°C. In particular, the shape of the precipitate particles and the amount of strain in the matrix, due to the precipitate, have been studied. The work described here is part of a wider investigation of factors that affect carbide precipitation in austenitic stainless steel," details of which are to appear elsewhere. RESULTS The present investigation can be conveniently split into two aspects of the strain-fields surrounding the matrix particles: 1) information derived from the strain-field which indicates the shape and habit plane of the precipitate particles and 2) the magnitude and sign of the strain-field. The Shape and Habit Plane of the TaC Precipitate. In the early stages of aging twin lobes (normally black F. H. FROES, formerly at the University of Sheffield, Sheffield, England, is Staff Scientist, Colt Industries, Crucible Materials Research Center, Pittsburgh, Pa. D. H. WARRINGTON is Lecturer, Department of Metallurgy, University of Sheffield. Manuscript submitted November 1, 1968. IMD on white background, i.e., for the deviation parameter, S > 0) that indicate the strained region of the matrix define the position of the particles by bright field transmission electron microscopy. The actual particles were not detected until they were approximately 120Å diam; below this size they were too small to be imaged in the electron microscope. This meant that particle growth that had occurred before this stage had to be inferred from the matrix strain-field contrast. In all cases when diffraction effects were observed from the precipitate particles, a cube-cube orientation relationship (i.e., (llO)ppt Il<llO>matrix and {1ll }ppt {III} matrix) existed between the precipitate and the matrix. From the matrix precipitate particles lying along edge-on {111} planes (e.g., at A, Fig. I), the precipitates are seen to be plate-like with their diameter being roughly 18 times their thickness after 5000 hr at 650°C. However, the exact shape of the particles cannot be determined because of the masking effect of the strain-field contrast. If a dark-field micrograph, using a precipitate reflection, is studied, Fig. 2, a number of the projected images of the TaC particles [on the (110) foil surface] apear to have straight edges parallel to projected f111) planes. Thus, it appears that in the later stages of aging the TaC particles are plate-like with some tendency for the edges of the plate to be bounded by the matrix close-packed {ill} planes (though the general shape of the particles in the plane of the plate is circular and thus the "diameter" of the particles has a real physical significance). It should be noted that the bands of fine discrete particles observed in Figs. 1 and 2 are not the matrix precipitate discussed in this paper but are precipitates associated with extrinsic stacking faults3j4 occurring on (111) matrix planes. **£** ****** \ *x 23 Fig. 1—18/12/2~a/0.1~ alloy. Solution treated at 1300°C for 1 hr, water quenched, and aged 5000 hr at 650°C. The (112) directions shown are the traces of the e&e-on (111) planes. Foil normal [110]; operating reflection (331); bright field micrograph.

Jan 1, 1970

By E. R. Buchanan, R. E. Reed-Hill

Cylindrical magnesium single crystals were deformed in torsion. The axis of torsion was the basal pole. Five crystals were deformed to different strains between 0.08 and 1.03 and then sectioned in order to determine their dislocation densities using the transmission electron microscope. The work hardening rate of all specimens was at least an order of magnitude higher than that normally associated with easy glide in a tension test and comparable to that obserzed in stage B of a tension test. The correspondence between stage B in a tension test and the initial stages of a torsion test is believed to result from the fact that in both cases deformation occurs in a structure containing roughly equivalent densities of the dislocations associated with the three basal slip vectors. THERE are three basic ways of changing the shape of a crystal using slip dislocations. The crystal can be sheared along a slip direction in a slip plane; it can be bent about an axis in the slip plane normal to the slip direction; and, if the slip plane contains multiple slip directions, it can be twisted or rotated about the slip plane normal. Of the three processes, generally known as translational, flexural, and rotational slip, only rotational slip has not been extensively investigated. The object of the present research was to obtain basic information about this phase of crystalline plasticity. This paper is concerned with some aspects of the stress-strain curves obtained by twisting magnesium crystals about their basal poles. Magnesium was selected for four reasons. One, its recovery rate at room temperature is relatively low. Two, single crystals may be easily grown. Three, at room temperature the critical resolved shear stress for basal slip is about two orders of magnitude lower than that for nonbasal slip, so that rotational slip might be expected to occur primarily by basal slip. Finally, relationships between flow stress, shear strain, and dislocation density have been determined for tensile deformation of magnesium crystals,&apos; thereby providing a basis of comparison for the torsional results. EXPERIMENTAL PROCEDURES Crystals were grown from 0.5 in. diam extruded sublimed magnesium rod furnished by the Dow Chemical Co. who reported that it contained in weight percent less than 0.0003 Al, 0.01 Ca, 0.01 Cu, 0.0012 Fe, 0.001 Mn, 0.0005 Ni, 0.003 Pb, 0.001 Si, 0.01 Sn, and 0.02 Zn, with the balance magnesium. All crystals were grown in a dried argon atmosphere using Jill-son&apos;s2 modified Bridgman technique. Two different methods were used to obtain crystals with the basal plane normal to the specimen axis. These included direct growth from seeds of the proper orientation, and spark machining (trepanning) of 0.5 in. diam cylinders from larger (1.5 in. diam) randomly grown crystals. The crystals thus produced were polished in a 20 pct HC1 water solution and then etched in a 1 pct HC1 water solution to develop etch pits lying in rows parallel to the basal plane trace. The crystals were then revolved about their axes on the stage of a low-powered microscope. Torsion specimens were prepared only from those crystals whose axes were normal to the rows of etch pits. It is estimated that this simple orientation method was accurate to about 51 deg. 1.625 in. long cylinders were next cut from these selected crystals and then acid machined in a 20 pct HC1 water solution into torsion specimens with a 1 in. long by 0.30 in. diam reduced gage section. Following this, they were annealed in air at 400°C and furnace cooled to room temperature. The specimens were given a final polish in a 10 pct HC1 water solution, rinsed in ethanol, dried, and cemented into brass grips with an epoxy resin. In addition to the torsion specimens, several tensile specimens with their basal planes at 45 deg to the stress axis were also prepared with similar dimensions except that the gage sections were increased to 4 in. in length. The torsion specimens were tested in the apparatus

Jan 1, 1970

By M. Deighton, R. N. Parkins

The metals Cd, ,Wg-, Sn, TI, Zn, and Zr reach a peak hardness after a criticfir1 deformation by rolling- and then soften with fwther rolling-, thereby exhibiting wovk softening. Optical metallography on Cd, Mg, and Zn shows that work softening is accompanied by a change in grain size occurring during deformation. The creep of zinc from -1l° to +60°C at stresses in the range of 7.9 to 17.3 kg per sq mm is given by € = e0 -t- Bt + Kt +at6. The third and second rate constcints are related by the equation a = K~ K6 and their stress and temperature dependence can be represented by the equations K = A, . exp - (u, - Bu)/kT. A model based upon the stress activated glide of sub-boundaries is proposed which qualitatively accounts for the metallog-raphic observations. Expressions, which are in reasonable quantitative agreement with the ex-pe~inzental observations, are derived for the creep of zinc. THE term "work softening" has been used previously by Polakowski1 and by Cottrell and stokes2 to describe phenomena where further strain of a deformed material leads to a decrease in flow stress. In both cases, however, the conditions were changed for the second straining. Here, the term "work softening" is intended to refer to a decrease in flow stress after continued straining in the same direction at the same temperature: work softening is the antithesis of "work hardening". Work softening of zinc was reported by chadwick3 and in discussion of that paper Jenkins4 indicated that cadmium also work softens. More recently work softening has been reported5 in two magnesium alloys, -99.5 pct Mg. Chadwick found that the hardness, 0.2 pct Proof Stress and the UTS of electrolytic zinc all increased with progressive cold reductions up to 30 pct and then progressively decreased with further rolling. Gay and Kelly6 used a back-reflection X-ray technique to study the effect of cold rolling zinc and found that although deformations greater than 2 to 5 pct reduction in thickness produced some recrystallized grains, deformations greater than 40 pct caused com-plete spontaneous recrystallization. At deformations greater than 60 pct the material was found to consist solely of recrystallized grains, -20 pm diam, the size of which decreased with increasing reduction and was much less than the initial grain size of the annealed material (-300 pm diam). Similar results were also reported for cadmium, tin, and lead.6 Gay, Hirsch, and Kelly&apos; suggest that these experiments indicate recrys-tallization takes place when the dislocation density exceeds a certain value. However, no measurements of MATERIALS AND EXPERIMENTAL PROCEDURE The purity of the metals used in this work is indicated by the following figures: Zn (99.99); Cd (99.94); Mg (99.95); T1 (99.99). The zirconium was iodide crys tal bar with a probable purity of about 98 pct. The metals were obtained in the form of 0.25 in. thick strip or 0.425 in. diam rod by various fabrication methods and then annealed to ensure complete re-crystallization. Hardness-deformation curves were obtained at room temperature by rolling 4 in. thick strip under conditions which left a surface adequate for diamond pyramid hardness tests immediately after rolling. The hardness was taken as the niean of five impressions made using a 5 kg load and the time elapsing between rolling and making the last impression never exceeded 5 min. The zinc specimens for creep testing were from 3 by 3 by 4 in. cast slabs which were rolled to 0.10 in. thickness starting at 350°C and finishing cold. The resulting strip was cut into pieces 1 in. wide and annealed in batches. With suitable choices of annealing temperature between 100" arid 400°C five different grain sizes varying from 4.54 x 10&apos; to 3.03 x l05 grains per sq cm (530 to 20 um diam) were obtained. Creep tests were done in compression using a sub-press, based on a design after Ford,8 in which the strip is compressed between dies 0.100 in. wide under conditions of plane strain. Since there is no lateral spread of the material, the area of contact between the dies and strip remains constant throughout the test and the application of a constant load, using the load maintaining device of a hydraulic testing machine, resulted in a constant stress. Covering the dies with strips of P.T.F.E. reduced frictional effects to a minimum. The creep strain was obtained by measuring the travel of the crosshead of the testing machine to a sensitivity of 0.1 pct reduction in thickness. The complete subpress assembly was contained in a steel box and for tests above the ambient this was filled with liquid paraffin and heated electrically. Temperatures below the ambient were obtained with a cooling mixture of acetone and solid carbon dioxide in the box. The liquids were stirred and the temperature of the specimen, which was controlled to ±0.5"C dur-ing a test, was measured by a thermocouple placed near the dies. Compression testing of cylindrical specimens was also carried out in the subpress using hardened flat discs separated from the test material by P.T.F.E. sheets which obviated barrelling of the specimens. Various initial strain rates were supplied by the hydraulic testing machine, and the deformation was measured by a clock dial gage resting on the cross-

Jan 1, 1970

Over and above the technical support arid consulting work described in the preceding Parts of this Volume, ADL staff also provided a wide range of additional technical assistance to the Bureau on an ad hoc basis over the course of the contract, and particularly in 1973. Some of these assignments were on tasks that temporarily assumed a high priority at PMSRC, requiring a fast response, while others were more suited to conventional schedules but on communication and location topics less directly related to those in the preceding Parts. Chapter I briefly describes some of the diverse short-term assignments while Chapters I1through V treat assignments on the other topics. I SHORT-TEXM ASSIGNMENTS A sampling of short-term, fast-response assignments undertaken on mine communications and miner location for PMSRC during 1973 are given below. These assignments included technical reviews, discussions and recommendations related to the theory, experimental data, designs, and hardware implementation of experimental CW and pulse miner location EM transmitters; preparation of technical performance specifications for a miniaturized preproduction prototype CW electromagnetic location transmitter; review of specifications for a seismic signal detection experimental study; participation in technical discussions and experiments with PMSRC and equipment suppliers regarding the UHF radio/radiax-cable communications installation in the Bruceton mine; participation in an informal conference to discuss mine communication and monitoring needs and preferences with representatives of the Bureau, mine operators, and equipment manufacturers; participation in technical discussions with representatives of a U.S. mine operator and CERCHAR* concerning the characterization of faults on trolley lines and means of improving their rapid detection;** recommendation of simple signal, noise, and ground fault measurements on mine phone lines; review of an inexpensive automatic telephone dialer; preliminary discussions regarding the feasibility of adapting and assembling a collection of available telephone industry carrier equipment for installation and test in an operating coal mine; evaluation of a proposed call alert mine paging system; review of hardware designs and future experiments for a mine communication sled; design critique of a proposed six-channel narrow-band FM voice modem for carrier communication on the mine phone line; preparation of technical performance

Jan 1, 1974

By Francis Crowley

Elementary concepts of seismic wave properties are reviewed to establish a framework for discussing seismic noise and its suppression. A liberal number of references is included for those who wish to pursue the topic in detail. A base motion noise level is established for a single surface seismometer. It is argued that simple array processing and seismometer burial should regularly permit us to approach this base noise level which is found in areas free of conspicuous man-made seismic noise sources. The sensitivity of the base seismic level to a number of common disturbances is presented. Solutions that promise to hold the "effective" seismic noise at a site near the base level are given for acoustic, meteorological and fixed local surface sources. Guidelines are suggested for controlling other local man-made sources, e.g. vehicular traffic, by keeping them at sufficiently large distances away from the seismometers to keep noise at permissible levels. These guidelines are speculative and conservative. They should be the subject of future study. The ability to process against general local activity, drilling, and intra- mine sources is limited. Certainly no dramatic gain is to be expected. When strong man-made and/or intramine noise sources are not controllable, detection may well be impossible to achieve, unless the seismometer can be moved close enough to the suspected miner position, i.e. via very deep holes, to compensate for the likely vast differences in strength of the miner signal and the uncontrollable man-made noise sources. However, many intramine sources, e.g., falling water, rock bursts, explosions, etc., may well preclude the existence of a hale miner in their vicinity, and therefore any need to attempt detection of a miner at such locations. The following recommendations are made to enhance the detection and location of a miner signaling seismically. They are: 1. Seismometer burial in slim holes. 2. Narrow band detection, using multiple narrow band filters to cover the likely signal band. 3. Broadband recording and analysis for time-of-arrival estimation.

Jan 1, 1974

The first phase of our work for PMSRC on this contract was devoted to a comprehensive and in-depth assessment of electromagnetic (EM) noise measurements and data taken by several contractors for use in the design of operational and emergency mine communications. Pertinent measurements and data of other selected investigators were also included in the evaluation. This assessment treated the measurements and instrumentation used, the data analysis and presentation methods, and the utility of the final results. This phase concluded with the identification of the most useful results and methods, the remaining data gaps, the contractor most qualified to fill these data gaps, and the definition (with PMSRC and this contractor - NBS, National Bureau of Standards) of a follow-on noise measurement program, instrumentation system, and data processing methods tailored to obtain the necessary but missing noise data. A partial bibliography of references related to electromagnetic and seismic noise and propagation in the frequency bands of interest was also compiled during this first phase. The body of this Part of the final report presents a summary of the findings of our EM noise assessment, together with detailed recommendations regarding the new noise measurements to be taken and the instrumentation and data processing methods to be used. This work was done during the latter part of 1971 and the early part of 1972. During subsequent phases of the contract ADL was asked to perform on-going evaluations of the continuing program of electromagnetic (EM) noise and propagation measurements made by Bureau contractors, and to utilize pertinent data from these measurements to make performance estimates for

Jan 1, 1974

This Volume documents the Phase 111 effort on the Seismic Detection and Location of Isolated Miners on Contract H0122026 undertaken during the fall of 1972 by a task team composed of ADL staff and several seismic consultants. The team was assembled specifically to work together on complementary tasks, at an accelerated level of effort for four months, to meet the Bureau of Mines&apos; time schedule for obtaining independent, objective, technical judgments regarding seismic methods and systems for detecting and locating isolated miners. The impetus for this work resulted from a compilation and analysis, during the first half of 1972, of new experimental data obtained from a series of in-mine field tests conducted by Westinghouse Corp .+ using the CMRSS* interim seismic location system. The Bureau of Mines took advantage of the availability of these new data to reassess the potential and limitations of various seismic methods and systems, and to direct its seismic system improvement program accordingly. ADL assisted the Bureau in this reassessment by drawing on the skills of seismic consultants from industry, universities and government, to supplement the skills of the ADL project team. The consultants were principal resources of broadly-based and detailed technical expertise in the areas of seismic signal-source and signal-propagation characteristics, natural and cultural seismic noise, seismic sensors and field instrumentation, seismic signal and data processing for detection and location, and overall seismic system utilization in the field under operational emergency conditions. Specifically, the participating consultants were: F. Crowley, Air Force Cambridge Research Laboratories ; W. Dean, Teledyne Geotech, Alexandria Laboratories; R. Greenfield, Pennsylvania State University; J. Kuo, Columbia University; D. Peters and R. Crosson, University of Washington; and F. Pilotte, U.S. VELA Seismological Center. The principal ADL participants were J. Ginty, R. Lagace, M. Roetter, and R. Spencer.

Jan 1, 1974

This Part describes a mine pager phone to public telephone interconnect sys tem that permits mine paging telephones to be selectively interconnected with the public telephone system, as illustrated by Figure 1. This interconnect concept was first conceived and demonstrated in breadboard form by H. E. Parkinson of Industrial Hazards and Communications, PMSRC, as one means for providing improved emergency and off-hours communications. The third-generation prototype unit described in this Part was designed and fabricated by Arthur D. Little, Inc. This unit is a small desk-top or wall-mounted unit that connects directly to both the public telephone line and the mine pager phone line, and requires no modifications to either the public dial telephone or mine pager phones. As part of this task, ADL also built, under a very compressed time schedule, a second-generation prototype unit suitable for reliable demonstration of the interconnect concept during the Bureau&apos;s technology transfer seminar on mine communications in March 1973. * A major objective of the design of the third-generation unit described in this Part was that it be compatible with present mine pager phone systems utilizing DC voltage on the mine phone line to activate the phone loudspeakers. Therefore, this unit was designed to operate in a push- to-talk, push-to-listen mode that accommodates the inherent design differences and operation modes of the mine phones of different manufacturers. Though this push- to- talk, push- to-listen mode of operation may seem slightly unusual at first sight, we have found it is easily learned by new users. However, mine phone manufacturers wishing to expand their product lines with such an interconnect system will probably find it to their advantage to customize the design of this system to their particular mine phones, thereby utilizing the unique attributes offered by their individual product lines. This customization should not be difficult, and Section III below suggests some of the features that can be easily added to future designs. Detailed parts lists and circuit schematics for the present third-generation proto- type system can be obtained from the system manual submitted to PMSRC and placed on public file.

Jan 1, 1974

By John T. Kuo

The miner&apos;s seismic source strength can be approximately estimated on the basis of a single force acting in an infinite medium. Because of the uncertain- ty involved in estimating the amount of conversion from mechanical energy to seismic energy, the source strength thus estimated may be in error by as much as a half-order of magnitude. Calculations of wave transmission must take into account geometrical spreading, dissipation of energy by internal friction, and energy partition due to reflection and refraction of waves impinging on inter- faces in the layered earth. Theoretically derived peak-to-peak particle velocities in microinches per second (PIPS) are given for two models ; viz: (i) 50-feet thick and (ii) 100- feet thick 4000 ft/sec layers with Q = 20, overlying a half-space of 10,000 ft/sec material with Q = 5O;for the cases .of a hammer blow and a timber impact, at the frequencies of 50 Hz and 100 Hz. Comparison of the theoretically derived peak-to-peak particle velocity with experimental data taken at the Copper Queen Mine indicates that the theoretical particle velocity may be overestimated. A discussion of the distortion of seismic wavefronts by mine tunnels indicates that it is unfavorable to use a seismic source impact on the floor of the tunnel, since deceptive delays in arrival time are liable to occur at the surface. A program of parallel theoretical and experimental work is required to clarify uncertainties still associated with the nature and strength of the miner&apos;s seismic source signal which cannot be resolved within the approximations of this work. Its major components include theoretical investigations of the (1) Wave diffraction and scattering of an impact source on a face of a cylindrical cavity. (2) Impact of an elastic object on an elastic medium.

Jan 1, 1974

By Frank Pilotte

Proper design characteristics for a seismic system to locate miners during a mine disaster are considered in terms of a total system concept. Field hardware, processing equipment, operating personnel, deployment, training, and supportive R and D are necessary elements of the total system. Each of these elements is discussed and an indication given as to the requirements necessitated by each one. Hardware must be portable, rugged, and fieldworthy. Processing equipment must be simple to operate, expandable for future processing improvements, and ruggedized for field use. A small well-trained team must be available for quick response in times of emergency. Alternative deployment procedures are necessary to allow for a variety of situations including both ground and air delivery. Supportive R and D is used to support training and upgrading of the system.

Jan 1, 1974

This part of the final report treats some problems related to coal mine carrier frequency communication systems using the trolley wire/track transmission line. This work was undertaken for a brief period of time during the summer of 1972 to help understand, quantify, and improve some of the trolley wire carrier system behavior observed and/or predicted. Calculations and estimates of transmission line characteristic impedance, inductance and capacitance per unit length, mine motor loading effects, parallel line effects, and connection impedances are presented in Chapter I. Chapter II treats the design of r-f isolators for reducing the undesired and troublesome r-f loading that mine motors present to the trolley transmission line. Chapter III treats a diversity method for combatting standing wave nulls. I. CALCULATIONS RELATED TO TROLLEY WIRE COMMUNICATIONS A. ESTIMATION OF INDUCTANCE AND CAPACITANCE PER UNIT LENGTH OF TROLLEY LINES To estimate the L and C per unit length of trolley lines, we use the eccentric line model of Section G of this Chapter, "Characteristic Imped¬ance Estimates for Mine Trolley Lines." The capacitance per unit length for an eccentric line is given by (1)

Jan 1, 1974

By Roy Greenfield

During the detection phase, several procedures can be used to improve the signal-to-noise ratio (SIN) . • Subarrays of up to 10 seismometers should be used. The apparent failure to obtain improvement in SIN in the Westinghouse subarrav work is probably due to excessive noise in the electronics. The spacings needed for sensors in the subarray must still be established. • The sensors should be buried. Even burial to a few feet will probably give appreciable reduction of noise. A deeper burial will probably further reduce the noise; and, if the seismometers can be put below the weathered layer, the signal level will probably be increased. The reduction in noise by burial will be especially effective during high noise periods due to wind or rain. • Before attempting detection, the waveforms should be bandpass filtered. The bandpass should go from 25 Hz to an upper frequency of 100 to 200 Hz. Further measurements with a low noise system must be done before the signal-to-noise ratio can be determined for the 100 to 200 Hz range. Any narrow band noise should be removed by notch filters. • If noise levels differ among seismometers of a subarray, weights inversely proportional to the noise power should be applied to the seismometers. • Automatic methods of screening data for possible signal arrivals should be developed, but the final determination that the signal on a subarray output appears to be from a miner should be made by an analyst. Detection of "signal" on several subarrays should be required for positive identification. In the location phase, after detection: • If repeated signals are received, they should be coherently added (stacked) to give as good a SIN as possible for use in determining signal arrival times, to be used in location computations. The miner should, if possible, repeat the signal 25 to 50 times.

Jan 1, 1974

Coaxial cable structures form the subject of substantial theoretical and experimental investigations either directly related, or which can be extrapolated, to the communications needs and environments of U.S. coal mines. Communication systems based on "guided" waves, of which "leaky" coaxial cables are one implementation, are attractive candidates for providing a range of communication functions primarily along haulage ways, and possible also within sections up to the working face. (However, there are still strong reservations as to whether a practical coaxial cable sys tem could provide sufficient communications coverage within a section. ) In this Part, we present the results of some theoretical calculations of the performance of leaky coaxial cable communication systems. We also analyze the applicability of the theoretical and experimental results obtained by other researchers to the needs of U.S. coal mines. In particular, this investigation has been focused on the utility of relatively low cost, conventional, flexible, coaxial cable at frequencies covering the LF through HF bands and extending into the lower part of the VHF band, as opposed to relatively high cost, special semi-rigid, coaxial cable* at frequencies in the VHF and UHF bands. There are three major design alternatives for coaxial cable communication systems considered in this chapter: • Base station feeding a coaxial cable with high surface transfer impedance (holes in outer conductor, e.g., braid construction). • Base station feeding a coaxial cable with repeaters (U.K. experiments). • No base station, direct communication via a coaxial cable with periodic radiative structures.

Jan 1, 1974

By David C. Peters, Robert S. Crosson

A method of error analysis has been applied to the location technique of non-linear least squares iterative inversion in order to evaluate the resolving power of several seismic array configurations with various assumed earth models and errors and inaccuracies in arrival times. The results obtained demonstrate that lateral accuracies of location are improved significantly when the depth of the miner is known. Lateral location to within 100 feet appears achievable in many instances. If it is possible to refine earth models significantly beyond what has normally been assumed in this work by the use of on-site data, or if the mine is shallow (300 feet or less), accuracies of-about 30 feet or so may be attainable. Inaccuracies in earth models of about 5% are found to contribute much more heavily to these location inaccuracies than errors of a few milliseconds in picking arrival times; however, arrival time errors of 15-20 ms or above will dominate these model inaccuracies. The expected accuracy of location is found to fall off very rapidly as the miner moves outside the array. The strength of this effect depends markedly upon the geometry of the array configuration and can be reduced by careful design. Also, as the size of the array is increased, expected location errors within the array are not altered much, but continue to match the error associated with the smaller array over a larger area (assuming that all stations can still pick up the miner&apos;s signals). Better location accuracy, especially with respect to depth control is achievable in an earth where the velocity is depth-dependent (increasing with depth) than in one which is homogeneous. This is an advantage since the

Jan 1, 1974

In this Part, we have included copies of the flip charts and overhead projector viewgraphs used in the two briefings we conducted as part of this seismic detection and location task. The first one was an overview and problem definition briefing given to the seismic consultants on September 7, 1972. The second was a formal oral presentation of study results to technical staff members of the Pittsburgh Mining and Safety Research Center on November 21, 1972.

Jan 1, 1974

By Roy Greenfield

Estimates are given for the distance from a seismometer at which a miner can probably be detected. The procedure in making these estimates was to first establish the natural noise levels at the output of a surface seismometer for the 25 to 100 Hz frequency passband. The noise levels give the range of values which may be expected in areas with no man-made noise. For each noise level, we give the detection threshold which, when exceeded, indicates that a signal has been received. Based on the signals recorded by Westinghouse, curves are given which show the peak signal amplitude as a function of source- to-receiver distance (slant range). Curves are given for the Westinghouse seismic thumper, a 50-pound timber, and a sledge. For a given type of source, the receive signal strength depends more strongly on slant range than on any other factor. However, there is approximately a five-to-one scatter in the amplitudes. Thus, further study of factors affecting the signal amplitude might allow better estimates to be made for any particular geological setting. Combining the signal amplitude with the detection thresholds for the different noise conditions gives the distances at which a miner should be detected. These are given in Table l* below. [ ] The text also gives the increase in detection ranges which should occur if steps are taken to increase S/N by 10 dB. We feel that 10 dB is a conservative estimate of the improvement possible. During an actual rescue operation, the seismic crew and system should be capable of making on-site estimates of their detection capability, based on measurements of the site noise, and upon the best available estimates of the

Jan 1, 1974