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By D. M. Schuster, E. Scala

The elastic effects occurring in the matrix of a composite reinforced by discontinuous fibers were studied by means of photoelastic techniques. A hirefringent plastic was employed as the matrix material with high-strength a Al2O3 whiskers as the reinforcing fibers. It was found that for whiskers aligned parallel to the tensile load direction: (I) Matrix reinforcement occurred along the length of the whisker to within about 5 diameters of the whisker tip for a length to diameter ratio, L/D, of 40. (2) Significant stress concentrations were created in regions immediately surrounding the tips; the fine as-formed tapered ends exhibited the minimum stress concentration whereas the square-ended whisker produced relatively high values, K r 2.5 for L/D = 40. (3) The axial and radial stress distributions could he determined quantitatively; the stress distribution at the whisker-matrix interface was in general agreement with theoretical calculations. (4) The highest source of stress concentration occurred at points of fracture in whiskers which had ruptured after incorporation into the composite. Whiskers aligned perpendicular to the load direction neither reinforced nor caused appreciahle stress concentrations in the matrix. ThE properties of composites have generally been formulated empirically on the basis of macroscopic tests. There are still many questions concerning the mechanical and chemical interactions occurring at the interface between the reinforcing fiber and its matrix. Continuously reinforced plastics and dispersion-hardened metals represent the two extremes of composite reinforcement. Whether artificially produced or formed in situ, the whisker composite falls between these two extremes and is an example of discontinuous fiber reinforcement. The effect of fiber shape, size, surface condition, and end configuration on the stress distribution in the matrix is important since the presence of stress concentrations, especially in any high-strength, thin-wall structure, could become the cause of catastrophic failure. DOW,' in his theoretical discussion of discontinuous fiber reinforcement, has pointed out that appreciable stress concentrations occur at the tips or ends of the reinforcing fibers. It is the purpose of this study to examine directly, by means of the photoelastic technique, the stresses which occur in the vicinity of a discontinuity or whisker tip and to measure qualitatively and quantitatively the effects of whisker geometry when embedded in a birefringent matrix material. The use of sapphire (a A1,O3) whiskers was decided upon as the reinforcing agent because of their high elastic modulus (E- 60 X 106 psi) and in some cases strengths in excess of one and a half million psi. Sapphire whiskers are of further practical interest since they retain large fractions of their strength up to temperatures approaching the melting point (3720oF).2 The whiskers were grown, by the vapor-phase reaction commonly employed,3 as part of this study to insure a physically uniform supply. Tensile and bend tests were performed to verify that the whiskers were of the expected ultra-high strength. The high-strength whiskers can be identified and selected from the combustion boats by surface perfection, shape, and size; otherwise, strength values can vary by a factor of ten or more. Macroscopic defects are quite common on the surface of large bladed whiskers and the principal experiments were conducted with hexagonal whiskers of about 0.002 in. diameter and lengths ranging from 0.1 to 0.4 in. Upon completion of these two phases of the experiment, several birefringent resins were evaluated. A plastic, developed by Zandman,4 which is supplied by the Budd Co., was found most suitable and was used as the matrix material for the whisker composite throughout the study. It has a sensitivity of 60.5 lb per in. order, calibrated in tension and cures without introducing residual stresses. Young's modulus for this matrix material is 430,000 psi in the fully cured condition. Since good wetting and bonding between the sapphire and the matrix material is essential to the interpretation of the results, a wettability test was performed. The contact angle was measured to be 168 deg where perfect wetting is defined as 180 deg; therefore, the Budd Plastic wets the sapphire

Jan 1, 1964

By C. Graeme-Barber, R. L. Bell, T. G. Langdon

An analysis is made of the formulas and ,methods used to estimate the contribution of grain boundary sliding to the overall strain of a polycrystal. The errors involved in the approximations and/or ,mistakes in earlier work are assessed quantitatively so as to make possible the critical use of previously published data. SINCE it has been found that, under conditions of very slow creep, the strain due to grain boundary sliding (?gb) may contribute as much as 80 pct of the total creep strain,1,2 it is obviously important to have reliable methods for estimating this grain boundary strain. In two recent papers Stevens3,4 has drawn attention to the pitfalls encountered in assessing ?gb. He criticizes 1) the assumptions made in the derivation of some of the formulas for ?gb, and 2) the indiscriminate averaging procedures used for obtaining the quantities substituted in these formulas. These and further criticisms of earlier work are mostly valid. Unfortunately the only formulas and procedures recommended are either impossible or very difficult to apply in practice. Furthermore no attempt is made to assess the errors involved by the earlier approximations or mistakes, and so it is not possible to make critical use of any of these early dab. The present article attempts to improve on these shortcomings by reference to empirical verification of easily applied formulas whose theoretical derivations involve some otherwise unjustifiable assumptions, and by a quantitative assessment of the errors in previous work. DEFINITIONS First it is necessary to define the terms and symbols to be used. The choice of symbols preferred here is a logical combination and extension of the v introduced by McLean5 and the u by Brunner and rant.' In Fig. 1 the two grains X and Y are displaced by the sliding vector AC. u is the component of sliding resolved along the stress axis, v is that measured perpendicular both to the stress axis and to the specimen surface, and w is that measured perpendicular to the stress axis but in the plane of the surface. Two angles define the orientation of the grain boundary: 8, between the stress axis and the surface trace of the boundary, and +, the internal angle on a longitudinal section cut perpendicular to the surface. In computing the strain resulting from the boundary displacement at all the in- dividual boundaries in a polycrystal the components u, v, or w are sometimes averaged along a longitudinal line (i.e., parallel to the stress axis), sometimes along a transverse line, and sometimes at randomly chosen boundaries. Averages obtained in these three ways are given subscripts 1, t, and r, respectively. Stevens rightly calls attention to the possibility of non-equiaxed grain shapes either at the start or at the end of deformation. In this article all values of numbers of grains per unit length will refer to measurements made before deformation. The subscripts 1 and t will be used for the number of grains per unit length obtained along longitudinal and transverse lines, r for that obtained by averaging along a number of randomly directed lines. FORMULAS FOR ?gb ?gt, as a Function of u. An obvious truth is that cgb can, in principle, be obtained by summation of all the v components at the boundaries intersected by a longitudinal line of known length I, viz.: where nl is the number of grains per unit length, parallel to the stress axis, in the unstrained specimen. There are assumptions in the analytic derivation of Eq. [I] due to Brunner and rant' but ~achinger' arrived at Eq. [la] by a rigorous method. Unfortunately the experimental procedure required by Eq. [ la] proves very difficult as boundary migration tends to obscure the points at which the longitudinal line meets the grain boundary and the errors on such measurements tend to be large, see Fig. 2. For example, on a specimen of Magnox AL 80 at a creep strain of 9.7 pct, 300 measurements of u obtained from the points of intersection of a longitudinal line with the grain boundaries gave ul = 8.95 ± 3.58 pm, or an error of ±40 pct, at the 95 pct confidence limit. These large errors due to migration may be avoided by measuring u from the separation of the segments

Jan 1, 1968

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By Charles Smeal, Robert J. Schafer, Max Quantinetz

Normally metal powders cannot be ground to sub-micron sizes because of welding and agglomeration phenomena. Through the use of selected grinding aids and grinding fluids, nickel and other metal powders have been ball-milled as fine as 0.1 It was found that certain inorganic salts are more effective grinding aids for metal powders than conventionally used surfactants. METAL and alloy powders are used to produce reagents, pigments, coatings, solders, brazes, and parts for industry by powder metallurgy techniques. They are also combined with refractory compounds to produce cermets and dispersion-hardened products. One of the interests at the Lewis Research Center has been to explore the potentialities of the dispersion strengthening process. Since the work of Ir-mann, many investigators have shown that the strength of dispersion-hardened products may increase with decreasing interparticle spacing.24 One approach to achieving small interparticle spacing is to combine fine refractory compounds and metal powders, preferably below 1 in size. In attempting to obtain fine metal powders, it was found that until very recently the best that could be obtained from commercial suppliers, particularly of ductile metals, was about 1.0 . Interest was therefore developed in providing finer metal powders for dispersion-hardening studies. Information obtained from the literature, from others working in the field, and from prior experimental work performed at NASA, led to a consideration of ball-milling as a technique to produce the desired materials. Some of the variables associated with ball-milling are the size, material, and nature of construction of the grinding container; the nature and amount of the grinding material and material to be ground; and the nature and amount of the grinding liquid and grinding aid, if employed, and the grinding time. In all ball-milling, welding and agglomeration can oc- cur as well as grinding. Because of the tendency of ductile metals to weld together, they are difficult to grind.5 The ultimate particle size obtained on grinding is generally the one at which the rate of grinding becomes equal to the rate of welding. To help delay welding and thus obtain smaller particle sizes, grinding aids are often employed. The principal objective of this investigation was to produce submicron metal powders by ball-milling the powders with selected grinding aids and grinding fluids. A secondary objective has been to attempt to explain the variations observed in grinding behavior by considering possible grinding mechanisms and correlating various parameters with grinding effectiveness. Three groups of ball-milling experiments were run; one in which the grinding aid was varied, a second in which the grinding fluid was varied, and a third in which the material being ground was varied MATERIALS, APPARATUS, AND PROCEDURE In the first group of experiments in which the grinding aid was varied Inco Carbonyl Grade B nickel powder initially 2.5 (all sizes refer to average particle size as measured by Fisher Sub -sieve Sizer) was used as the material being ground and 200-proof ethyl-alcohol as the grinding fluid. Surfactants, representative of typical organic structures, were selected as grinding aids. Inorganic salts used as grinding aids were chosen on the basis of the size and valence of their ions. Water soluble salts were used in order to facilitate their removal from the slurry after grinding. In the second set of experiments, grinding of the 2.5- Ni powder was tried in four different grinding liquids; water, cyclohexane, n -heptane, and methy-lene chloride. In this study seven grinding aids selected from those tried in the first group of experiments were employed. In the third group of experiments 200-proof ethyl alcohol was again used as the grinding fluid to mill Cu, Cr, Fe, Ag, and Ni powders of various initial particle sizes' All mill charges contained 300 ml of grinding liquid and 3000 g of 1/2 in. stainless steel balls. When inorganic salts were used as the grinding aid, 70 g of salt and 210 g of metal powder were employed, and with surfactants 6 g of grinding aid and 300 g of

Jan 1, 1962

By R. W. Hertzberg, F. D. Lemkey, J. A. Ford

The technique of unidirectional solidification has been applied to the A1-AI3Ni and A1-CuAl2 ezltectic alloy systems; the controlled microstructure of A1-A3Ni consists of parallel A13Ni whiskers emhedded in an aluminum matrix while the Al-CuAl2, system solidifies as parallel alternate lamellae of aluminm and CuAl2. Mechanical tests (tension and flexure) have shown that the particle-matrix interface bond formed during unidirectional solidification allowes for efficient load transfer from the matrix to the reinforcing phase. Strength and fracture characterstics of the alloys were studied as a function of phase orientation; the tensile strength of controlled Al-Al3Ni samples was 43,000 psi (three times greater than that of as-cast specime~s). The strength of the Al-CIA2, cutectic was studied as a function of lamellae-flexure stress-axis orientation using a microbend apparatus. A twofold increase in outer fiber stress was observed as the lamellae were rotated from a position of no reinforcing (perpendicular to the stress axis) to one of maximum reinforcing (parallel to the stress axis), The brittle reinforcing constituent in each alloy (A13Ni and CuAl2) was observed to he the nucleating phase for fracture. It is to be concluded from this investigation that unidirectionally solidified eutectic alloys have a potential use as reinforcing coniposite) materials. In a recent review article, Chadwick1 has described the work of many investigators in the area of controlled solidification of binary eutectic alloys. Thus far, more than twenty eutectic alloys have been unidirectionally solidified to produce structures consisting of two phases in the form of alternating lamellae or as whiskers embedded within a continuous matrix; in either case, the phases are aligned parallel to the growth direction. In particular, Kraft and Albright2 have shown that the Al-CuA1, eutectic alloy exhibits a lamellar microstruc- ture as a result of unidirectional solidification while Lemkey, Hertzberg, and Ford3 have studied the A13Ni whisker-aluminum matrix morphology in the A1-A13Ni system. Whether these alloys could exhibit reinforcing behavior would have to depend upon the strength and volume fraction of the reinforcing phase (AI3Ni and CuA12) and the nature of the bond between the reinforcing phase and the matrix. Hertzberg and Kraft4 have shown that the interface bond between chromium whiskers and a copper matrix in unidirectionally solidified Cu-Cr is particularly good while Lemkey and Kraft5 have reported chromium-whisker tensile strengths in excess of 1,000,000 psi. However, with the chromium volume fraction being less than 2 pct, no reinforcing behavior was displayed by the Cu-Cr alloy.6 In view of the encouraging results concerning the good interfacial bond and high strength of the reinforcing phase in the Cu-Cr system and preliminary mechanical test data reported by Lemkey et al.3 for the A1-A13Ni system, the A1-CuA1, and A1-A13Ni eutectic alloys containing 50 and 10 vol pct, respectively, of the reinforcing phase give promise of possessing mechanical reinforcing behavior. Based on this premise, the objective of the investigation was to study the strength and fracture behavior exhibited by these anisotropic microstructures. EXPERIMENTAL PROCEDURE Controlled Solidification Procedure. An extensive description of the technique of unidirectional solidification has been presented elsewhere.' However, the pertinent details for each eutectic system studied are discussed below. Al-A13Ni System. Several master heats of this alloy were prepared by vacuum-induction melting in an A12O3crucible and casting in SiO2 mold or by induction melting in alumina crucibles under argon. The initial heats were prepared from 99.99 pct A1 and 99.99+ pct Ni, while later heats used 99.999+ pct A1 and 99.99+ pct Ni. Specimens of these master heats were unidirectionally solidified using induction and resistance heating sources and argon atmospheres at growth rates from 1.1 to 28.7 cm per hr. The thermal gradients in the liquid were controlled in the range of 26" to 36°C per cm for these runs. Al-CuA12 System. The master heat and controlled

Jan 1, 1965

By R. D. West

Miscible displacenzent recovers all oil in the area contacted by the injected .fluid, whereas water or immiscible gas drives usually leave substantial amounts of oil as residual. However, the Door mobility ratios associated with a gas-driven miscible displacement cause the sweep pattern efficiency to be much lower than that obtained with water flooding. One way in which the sweep eficiency in a miscible displacement process can be increased is by decreasing the mobility behind the flooding front. This can be achieved by injecting water along with the gas which drives the miscible slug. This water reduces the relative permeability to gas in this area and thus lowers the total mobility. The main operating conditions for the simultaneous injection -vrocess are that a zone of gas exists between the miscible slug and the leading edge of the water and that a su,@cient amount of gas be injected with the water to form the pas volume which is being left in the water zone. Laboratory model studies have shown that the ultimate sweep pattern efficiency can be as high as 90 per cent for a five-spot flooding system. If gar alone is used as the driving medium an ultimate sweep-out efficiency of about 60 per cent would be obtained in the same system. I INTRODUCTION The miscible displacement processes are a step towards total oil recovery. Conventional gas or water drives usually leave 25 to 5.0 per cent of the oil as residual in the swept portion of the reservoir. This residual can be eliminated if the oil is driven by a fluid with which it is miscible. At some reservoir conditions natural gas will become miscible with the oil. This is the "high pressure gas process".' More often, the oil does not contain enough light hydrocarbons to cause the gas to become miscible with the oil at reasonable pressures. In these cases a small band of fluid which is miscible both with the oil and gas must be kept between them2. Less than 2 per cent of the reservoir volume of the slug material is needed to keep the displacement miscible. Both processes work in the same manner, recovering all of the oil in the portion of the reservoir contacted by the injected fluids. The only difference is the manner in which the miscibility between the oil and the injected gas is obtained. Previous publications have contained detailed descriptions of these processes.1,2,3,4 However, total displacement of the oil in the swept region does not guarantee an efficient recovery process. The amount of oil to be recovered is also determined by the fraction of the reservoir contacted by the flood. This fraction is largely determined by the mobilities of the fluids. (The fluid mobility is the permeability of the rock to that fluid divided by the fluid's viscosity, k/p). This. dependence of the fraction swept on the mobility ratio has been shown in previous studies. Fig. 1 shows the ultimate fraction swept in a five-spot system as a function of the mobility ratio. The small drawings show the location of the areas left unswept for two different mobility ratios. The ultimate fraction of the reservoir swept is here considered to be attained when the producing stream contains less than 5 per cent oil at reservoir conditions. THE GAS-DRIVEN MISCIBLE DISPLACEMENT Since there is no oil left in the swept region after miscible displacement the mobility in this region is very high. It is often 50 times the mobility in the unswept regions. This means that the fraction of the reservoir contacted by the injected fluid will be less for a gas-driven miscible displacement than for a conventional water or gas drive. For a five-spot injection system, water would contact the entire reservoir volume, and the low pressure gas would contact about 90 per cent of this volume, while a gas-driven miscible displacement would only contact about 65 per cent of the reservoir. This poor sweep efficiency often offsets the benefits obtained through miscible displacement. Fig. 2 shows what the recovery curves for the three processes might look like for a five-spot system. The curves show the fraction of the in-place oil recovered as a function of reser-

By H. Groeneveld, C. A. Connally, P. J. Hoenmans, J. J. Justen, W. L. Mason

A miscible displacement pilot using a slug of LPG driven by separator gas was conducted in the Cardiurn reservoir of the Pembina field. The injection pattern was a 10-acre, inverted, isolated five-spot. Upon completion of the LPG-gar phase, an experiment was conducted using a slug of water followed by gas. Calculated performance of the pilot is compared with actual performance. Equations are developed to calculate the distribution of LPG into zones of varying permeability, to estimate the progress of the flood at different times in the various zones and to estimate gas rates after breakthrough. The analysis indicates that permeability stratification was a dominant factor in controlling oil recovery and that oil was completely displaced from the swept pore volume. The results of the pilot indicated that miscible flooding is a practical means of pressure maintenance in this reservoir. The total recovery from the pilot area was good in spite of the early breakthrough of LPG. The effects of stratification were reduced by injecting a slug of water into the partially swept reservoir. INTRODUCTION The Pembina field,' located in Alberta, is the largest oil field in Canada and one of the largest in the North American continent. The reservoir is a stratigraphic trap producing from the Cardium sand. Neither bottom water nor free gas has been found. The recovery of oil by the natural depletion mechanism has been estimated at 12.5 per cent. Pressure maintenance studies of various areas have indicated that the recovery can be increased 21/2 times by water flooding, and a large area of the field is presently under water flood. However, reservoir studies of the North Pembina area indicated that miscible flooding might be competitive with water flooding. A pilot test was conducted to evaluate the performance of a miscible flood. A 10-acre, inverted, isolated, five-spot pattern was selected for the pilot. The pattern area was large enough to minimize wellbore fracturing effects and contained sufficient oil to provide significant working numbers. The performance of each of the four producers could be evaluated individually and compared. In the event of breakthrough in one direction, the effect would be isolated from the other producers. The use of a single injector minimized the volume of LPG required, and, because of the high mobility of gas, one well was sufficient to inject the necessary daily volume to replace the high rate of production. With four producers, the test could be completed in time for results to be evaluated, additional engineering studies to be made and a unit to be formed before the reservoir pressure in the North Pembina area declined below the bubble point. The pilot was located in an area developed on staggered, 80-acre spacing. The injection well was drilled at a regular location, while the four producers were drilled 467-ft north, east, south and west of the injector. Each quadrant and its associated producer were identified according to their direction from the injector— that is, north, east, south or west. The eight surrounding producers on 80-acre spacing were shut in to isolate the pilot area and provide for reservoir pressure observation. The pilot wells were completed using permanent-type completion techniques. After coring, casing was run through the pay section and cemented. Inside 51/2-in. casing, 2 1/2-in. tubing was hung. The wells were perforated opposite the Upper Cardium sand and lightly fractured. Fracturing volumes, rates and pressures were low to minimize the extent of the fractures. The fracturing treatments average 1,000 lb of 20-40 mesh sand in 700 gal of a low fluid-loss sand-carrying agent. Feed rates and wellhead fracturing pressures averaged 5.5 bbl/min at 2,535 psig, respectively. After fracturing, the productivity index was measured in each of the five pilot wells. The average PI of the four producers was 0.41 BOPD/psig drawdown. The measured PI'S were approximately the same as PI'S calculated from core analysis data, indicating that the fracturing treatments were just sufficient to overcome

By M. A. Childers

Recent work with controlled laboratory tests.' field experience and a new analytical approach indicate that casing centralization, pipe movement and relative rheological properties between the mud and cement (yield point and density) are the three controlling factors in successfu1 primary cementing of dual casing. Turbulent flow has been demonstrated to be unnecessary under the severe displace ment conditions of parallel dual strings of casing. Simultaneous reciprocation of dual casing in directionally drilled boreholes is highly dependent on centralization and on the rapid initiation of pipe movement once the casing has been run to total depth. Successful cementing of 30 out of 32 dual, 3%-in casing wells substantiated these conclusions. A review of 15 dual, 3 1/2-in. casing wells completed prior to the adoption of these principles disclosed only one success. Mathematical and graphical techniques permit the engineer to analyze and anticipate the success or failure of a cementing operation. Standoff, mud displacement and reciprocation can be analyzed mathematically and planned in deep, directional or straight boreholes by review of annular geometry, relative rheological properties between the mud and cement, and forces caused by caring weight, functional drag and differential sticking. Introduction The objective in primary cementing is to displace the drilling fluid with cement that will bond to the formation and casing to prevent communication through the annulus. The predominant cause of failure appears to be channels of gelled mud that remain in the annulus after cementing.1 '* Past investigations have noted many procedures that could improve the displacement process.2-' These procedures include centralization, chemical preflushes, mechanical mud cake removers, controlled flow rates in certain regimes, pipe movement an1 control of mud and cement properties. Not until recently have the effects of many of these procedures been isolated so that their individual importance could be determined. In a recent paper,' a comprehensive and analytical laboratory study of various factors controlling the displacement process concluded that there are three major factors in obtaining complete mud displacement by the cement slurry. 1. Good relative rheological properties between the mud and cement. The cement should be heavier and have a yield point and plastic viscosity higher than the mud being displaced. Buoyancy forces often can dominate the displacement process. 2. High degree of standoff or centralization. The more centered the casing, the greater the likelihood of complete mud displacement and removal. 3. Pipe movement obtained by rotation or reciprocation. Often unfavorable rheological properties between the mud and cement, and poor standoff can be compensated by pipe movement. This work demonstrates the compatibility of the latter concepts with field results extended to the more severe dual casing displacement process. Early Experience With Dual 3'/t-In. Primary Cementing Early slim casing completions in the West Delta Block 73 field, offshore Louisiana, included 17 dual 3%-in., 3 single 3% -in. and 1 dual 2% -in. casing installations. Table I provides data on these earlier wells. Usually, common Class A cement was placed across the pay zone and 12 percent gel cement was placed to a height of 500 ft above the highest productive sand. Centralizers (6%-in. OD maximum expansion) were placed two or three per joint on both casing strings from total depth through the completion intervals and at least one per joint for the remainder of the cement sheath. A number of techniques and procedures were attempted to improve cementing success. Casing was run simultaneously or separately with a number of mud conditioning and circulating techniques. Mechanical aids such as cement bonders, slmiding sleeves, turbulizers and various sizes and strengths of centralizers were used. Common and gel cements were mixed with fresh or sea water with a number of different additives to control retardation and dispersion. Cements were thinned and mixed at high rates to try to induce turbulent flow in the annulus. On one well the "slow flow" method was used." Perforating was accomplished with a jet orienting gun. Unsuccessful cement jobs were indicated by production of extraneous fluids or by pressure communication between zones. On test, five wells flowed water, four flowed sand and six had pressure communication with the other string or the 10%-in. casing. A total of 25 remedial squeeze ce-

Jan 1, 1969

By W. J. PRIESTLEY

WHEN during the war the Navy Department decided to build an armor-plate and gun-forging plant of its own at South Charleston, W. Va., one of the most important units of the equipment proposed was a 14,000 gross ton forging-press to be used for forging, bending, and rectifying battleship armor-plate and making hol¬low forgings for large caliber guns. A press suitable for doing this kind of work was put into operation in the fall of 1921 and was operated successfully on armor-plate and large forgings until the closing down of the ordnance plant following the Limitation of Armament Conference held in Washington, February, 1922. PURPOSE OF THE PRESS There are three methods by which armor-plate can be made, namely, hammering, forging, and rolling the ingot. Each method produces a different result in the mechanical working of the steel. The hammer was eliminated as impractical from an operating standpoint. The first armor-plate made in this country was worked under a hammer at the Bethlehem Steel Co., between the years 1891 and 1893, but was superseded by forging when the large press was completed in 1893. Harry T. Morris of the Bethlehem Steel Co. informs me that the 1.25-ton steam hammer began operations in 1891 and was in operation for about two years. The Carnegie Steel Co. and the Midvale Steel and Ordnance Steel Co. also forged armor-plate. Certain European manufacturers rolled the plates from large slab ingots, after removing the sink-head and giving the body of the ingot a light pass under a hydraulic press. While rolling accomplished more mechanical work on the surface of an armor plate, forging, on the other hand, resulted in a greater amount of work in the interior of the plate. Either type of equipment involved an enormous expendi¬ture, so it was deemed advisable to adopt the method which would make it possible to use the equipment for more than one purpose. Since g large rolling-mill could be used only for the single operation of rolling armor-plate, a press was decided on, for the reason that it might be designed so as to forge armor, as well as bend and rectify it, and also be used in the forging of ingots for large caliber guns, both in the form of hollow forgings and also solid shafts.

Jan 1, 1926

By D. W. Levinson, L. E. Tanner

DURING the course of an investigation of the zirconium-iron-tin system the zirconium-iron system was reexamined up to 55 pct* Fe. The alloys pre- visible melting3 and X-ray diffraction studies were made of samples of the alloys. The ferromagnetic properties of ZrFe2were determined by Professor P. W. Selwood* using a modified Faraday balance.4 The zirconium-rich portion of the phase diagram is presented in Fig. 1 and compared with the work of Hayes et al.1 The maximum solubility of iron in ß is somewhat decreased while the eutectic temperature is raised. There seemed to be no change in the eutectic composition of 16 pct Fe. Since the base material was so low in iron content, it was possible to establish the maximum solubility in a between 0.017 and 0.025 pct Fe at the eutectoid temperature. The observation of fine ZrFe, particles in the micro structure of a specimen of 0.012 pct Fe alloy quenched from 700°C indicated that the solubility drops below this composition at 700° C and lower. Further study was made of the intermediate phase ZrFe2. wallbaum5 identified the compound initially as ZrFe2 with a C 15 (MgCu2) structure, placing it at 55 pct Fe stoichiometrically. Hayes et al.1 believed they found the phase at about 47.2 pct Fe and called it Zr2Fe3 but reverted to ZrFe, in the discussion of their paper.6 Jordan and Duwez7 confirmed Wallbaum's work as well as finding the same single-phase structure to about 62.3 pct Fe or Zr0-61 Fe2-18. In order to establish the ternary phase relations in the zirconium-iron-tin systema the exact position of this phase had to be known. This was accomplished by X-ray diffraction, visible melting, and metallographic techniques. Elliott8 obtained a single-phase ZrFe2 X-ray diffraction pattern from an alloy of about 55 pct Fe. This was confirmed in the present study with an alloy of 54.81 pct Fe. However, extra lines (attributable to a or ß zirconium) were found in diffraction patterns of the 47.42 and 49.83 pct Fe alloys. The melting characteristics of these same alloys were studied by suspending 47.42, 49.83, and 54.81 pct

Jan 1, 1960

By Philip B. Bucky

THE Mining Methods sessions, one of which was run jointly with the Industrial Minerals Division, were fortunate in having a number of exceptionally fine papers. At the Tuesday session R. P. Smith presented the results of six years' experience with prepaid medical care for the employees of the Hollinger mine. It was felt that this paper was a real contribution to the cross field of mining-medicine, and the presentation was exceptionally well done. Olof V. Lindqvist acquainted us with the consider- able progress made in blast-hole diamond drilling in recent times, especially in Canada. The opening of a mine is always a matter of considerable interest and the description of the procedure and problems encountered in opening the Mather mine of Cleveland Cliffs Iron was presented by L. C. Moore.

Jan 1, 1944

A. SILVERMAN,* Pittsburgh, Pa.-Prof. Richards has described a very interesting process. In addition to the method described, electroplating and a number of other processes have been used. In one, the two metals were heated and united under hydraulic pressure; in a second, the steel was coated with an alloy, brass for example, and the molten copper cast around this. The process that I would like to bring to the attention of the metallurgists present consists simply of pouring molten copper, brass, or cupronickel around a clean red-hot steel billet. 'It is covered by the Roth patents. The 8-in. cylindrical billet containing about 70 per cent. steel (core) and 30 per cent. copper is hot drawn or rolled until several inches in diameter and afterward cold drawn or rolled to rod, wire of any desired diameter, or sheet. The wire is used for electrical conduits where conductivity and high tensile strength are required, also for the manufacture of cables and screen cloth. The sheet is employed for the manufacture of spouting, molding, shells, etc. The last application is particularly interesting. In testing rifle cartridges, which usually contain lead-filled copper noses, pine boards 1 in. thick, covered with ¼ -in. rawhide, are placed 1 ft. apart. The value of the cartridge depends on the number of boards penetrated by .the bullet. In government tests made with copper-coated steel noses (15 per cent. copper on either side of the steel) the penetrating power was found to be approximately double that of pure copper noses. The advantage of copper-coated steel over cupronickel lies in the fact that the- former does not require any special heat treatment during the punching. Rifle cartridges were prepared from copper-coated steel in a number of government arsenals. The value of the combination was attested by the awarding of a contract for the construction of a $3,300,000 plant. Unfortunately, the contract was signed on the day preceding the signing of. the armistice and was cancelled several days later. Tests were conducted for about 1 yr. before the contract was awarded to determine the value of this combination of metals. Since the war a number of cartridge and shell manufacturers have signified their intention of using copper-coated steel.

Jan 4, 1919

By Joseph C. Platt

IT is not the object of the present paper to give a description of the minerals found on Mine Hill, in Sussex County, N. J., nor even to touch upon all the forms of the ores named, but to place upon record and call to the attention of the Institute some interesting facts concerning them. In May, 1875, after the Dover meeting, some of the members visited this locality, and, no doubt, it is fresh in their memories, being one of the best known mineralogical points in our country. It will be only necessary to describe it very briefly. Mine Hill and Stirling Hill, in Sussex County, N. J., the former being at the village of Franklin Furnace, and the latter near Ogdensburg,-are the only localities in the State where zinc ores are found in workable quantities.* Mine Hill is the more northerly, and mineralogically differs from its neighbor, chiefly in having no hydrated ores to speak of, while at Stirling this deposit is considerable. At both points Franklinite, red oxide, and silicate of zinc occur in large quantities. Mine Hill lies on the east side of the Wallkill River, above which it rises to an extreme elevation of about 150 feet. On the summit the outcrop of the Franklinite vein appears, while the lowest worked points are perhaps 10 or 15 feet above the level of the stream. Corn¬mencing at the northern end, where the Hamburg Road crosses it, this outcrop runs along the northwestern brow of the hill a distance of about 2000 feet, in a general southwest direction, to a point where is a large, cavern-like opening, called the "Southwest Opening." " Double Rock," about the highest point on the hill, lies near the middle of this 2000 feet of outcrop, and over or near it passes a property line, to which allusion will hereafter be made. At the Southwest Opening the vein bends abruptly towards the east,-the angle between the two parts being perhaps 45°,-and this easterly branch continues some 700 feet. From the northern part of the Stirling Hill deposit to the southern part of the Mine Hill deposit is about two miles, and in this interval the vein carrying Franklinite * See New Jersey State Geology, 1868, p. 669.

Jan 1, 1877

By A. W. Schillinger

Drilling was not entirely satisfactory in the search for native copper in the Osceola amygdaloid footwall, for oreshoots mined were more continuous than drilling indicated. The Geophysics Dept of Michigan Technological University developed a portable induced polarization drill hole probe with a 3-electrode configuration and a sampling radius of 5 ft ±. A 20 ma current of alternately reversed polarity is pulsed at 3.5 sec intervals and readings are taken every 2 ft. Potential is read during the "on" cycle for resistivity determinations. During the "off" cycle, after 10 ms delay, the 1P potential is sampled for 10 ms and recorded. Resistivity (ohm-ft) and "S" values (mv/v) are plotted on semi-log paper. A lithologic log is plotted based on resistivity and anomalous S values noted. The low resistivity amygdaloid contains sills of high resistivity basalt. Verified by core logs, contacts between amygdaloid and basalt could be picked to ± 0.5 ft from resistivity alone. Lithologic logs of long-steel holes, based on resistivity, then replaced sludge logging. An S value of 30 mv/v was established as the lower limit of diagnostic 1P effects in mineralized amygdaloid and 50 mv/v as a threshold value for ore. Of 914 footwall zones drilled, 315 were probed yielding 203 anomalies. Success increased from 34% for drilling to 72% for drilling and probing. As checked by mining, 46 probe results were 78% correct. Failures were due to the instrument not detecting copper or to the misinterpretation of an anomaly. No false anomalies were found. During the past ten years, the Calumet Div. of Calumet &Hecla, Inc has conducted extensive exploration and mining in the footwall of the Osceola amygdaloid lode in the native copper district in Michigan's Upper Peninsula. In an attempt to delineate more clearly the extent and nature of high-grade footwall copper mineralization, 876 diamond drill and long steel holes aggregating slightly more than 47,000 ft have thus far been drilled from the accessible hanging-wall workings in the Osceola No. 6, 13, 14 and 15 shafts. Early in this program it became obvious, through inspection of footwall workings in progress, that due to the erratic and bunchy occurrence of the native copper in the footwall zone, the exploration drilling was failing to outline completely the extent of the oreshoots. Early drilling re-

Jan 1, 1964

The following specifications, proposed by a sub-committee of the American Society for Testing Materials, are still to be adopted and subsequently submitted to the International Association for Testing Materials. Standard Specifications for Pig-Iron and Castings. I. Analysis.—It is recommended that all purchases be made by analysis. II. Sampling.—In contracts where pig-iron is sold by chemical analysis, each carload, or its equivalent, shall be considered as a unit. At least one pig shall be selected at random from each two tons of every carload, and so as to fairly represent it. Drillings shall be taken so as to fairly represent the fracture surface of each pig, and the sample analyzed shall consist of an equal quantity of drillings from each pig, well mixed and ground before analysis. III. Allowances and Penalties.—III all contracts, in the absence of a definite understanding to the contrary, a variation of 10 per cent. of silicon, either way, and of .01 in sulphur above the standard is allowed. A deficiency of over 10 per cent. in the silicon, up to 20 per cent., and a further increase in sulphur up to .01 over the above allowance subjects the shipment to a penalty of 1 per cent. in the price for each element so affected. IV. Base Analysis OF Grades. —In the absence of specifications the following numbers, known to the trade, shall represent the appended analyses for standard grades of foundry pig-iron, irrespective of the fracture, and subject to allowances and penalties as above. Silicon Sulphur Grade. Per Cent. Per Cent. No. 1,...2.75 0.035 No. 2,.2.25 0.045 No. 3,........1.75 0.055 No. 4,.1.25 0.066 Cast-Iron Pipe and Special Castings. I. Description of Pipes.—The pipes shall be made with hub- and spigot-joints, and shall accurately conform to the dimensions given in Tables Nos. I. and 11. They shall be straight and shall be true circles in section, with their inner and outer surfaces concentric, and shall be of the specified dimeneions in outside diameter. They shall be at least 12 feet in length, exclusive of socket. For pipes of each size from 4-inch to 24-inch, inclusive, there shall be two standards of outside diameter, and for pipes from 30-inch to 60-inch, inclusive, there shall be four standards of outside diameter, as shown by Table No. 11.

Jan 1, 1905

By Galen H. Clevenger

Equipment for treating lead ores was added in 1905 to a copper plant which the United States Smelting Refining and Mining Co. had built in 1902 at Midvale, Utah, about 12 miles to the south of Salt Lake City. By 1906 the lead section of the plant had been rounded out and consisted of a 90-ton gravity concentrator, fifteen hand-rabbled reverbera-tory roasting furnaces, six blast furnaces, a briquetting plant for handling flue dust and fine ores, a regulus furnace for concentrating the low-grade matte made in the blast furnaces, and a baghouse. The copper section was later abandoned and the plant has been operated for many years exclusively as a lead smelter. Some 45 years had elapsed at the time this plant was built since the first attempts to smelt lead ores in the West, and lead smelting had become a large and profitable industry but fundamentally little that was really new had been developed, which could be embodied in a plant built in this period. Principles and tools to work with had remained much the same as those borrowed earlier from European practice. Capacities had been increased and there were mechanical improvements but hand charging was still in vogue and there was little attempt to recover suspended particles carried out with the furnace gases, beyond settling in flues, which usually was only partly effective for recovery of the coarser particles. Satisfactory roasting and preparation of the fine components of the charge were still partially solved problems. The Midvale plant of 1906 may be regarded as more or less typical of the smelting plant of this period for treating complex western lead ores as distinguished from the recovery of lead from the simple lead ores to the eastward. The operation of a concentrating mill directly in conjunction with a lead smelter was, however, not common practice. The ores treated in this plant have from the beginning come from mines owned and operated by the company or have been custom ores purchased in the territory tributary to the plant. The treatment of custom ores is an important service to the small producer who does not have sufficient tonnage to warrant a plant, and serves to increase the tonnage of the operator of large properties, thereby helping to reduce

Jan 1, 1937

By William Rawles

THIS report is the first of a series planned by The Mineral Inquiry, organized by the American Institute of Mining and Metallurgical Engineers to make factual studies of the world's mineral resources in their political and international relations. The efforts of The Inquiry are directed toward filling certain notable gaps in available information, without duplication of many other investigations touching this field which are being conducted by other organizations, public and private. Much of its work is indirect-suggesting topics for study by other individuals and organizations and aiding in their planning and correlation. The present report is designed to show the nationality of the commercial control of mineral resources, in addition to the geographic distribution of production by nation-in other words, the overlapping of political and commercial control. Detailed accuracy cannot be claimed for the figures presented. For some companies division of ownership by nationality has been very difficult to ascertain, as many companies are reluctant to dis-close the extent of their holdings in other corporations, and the impossi-bility of tracing all stock ownership is obvious. Also there are frequent changes in the distribution of stock control. The percentages given rep resent only the participation that has been identified definitely, even though it is known in some cases with fair certainty that larger interests exist, as, for instance, American participation in foreign chromite companies. In bringing together these figures we have had the cordial co-operation of the United States Bureau of Mines, the United States Geologi-cal, Survey, the Mineral Division of the Bureau of Foreign and Domestic Commerce, the Brookings Institution, and of many specialists connected with the mineral industries covered. The report does not cover the entire list of minerals: Coal, although it is one of the most important minerals, was omitted because not more than one or two per cent of the world's production comes from mines that are owned by companies foreign to the countries where the coal is produced. Others, such as gold, are omitted because sufficient data have not yet been accumulated. It is hoped that some of these may be covered in subsequent reports. It is not our purpose here to discuss the significance of the figures sub-mitted, but only to point out the general nature of the problems on which they have a bearing.

Jan 1, 1933

By J. R. Low, M. Gensamer, W. T. Lankford

THE problem of sheet metal formability is one which has received a vast amount of attention during recent years. In spite of the great amount of study and experimental work which has been devoted to this problem, many of its fundamental aspects are still not well understood. No generally satisfactory test has been developed which is capable of providing a reasonably adequate evaluation of sheet metal formability, particularly in borderline cases. Anomalies persistently arise in which a lot of supposedly satisfactory material exhibits excessive breakage when formed. This lack of suitable technological tests greatly hinders the design of new parts and the substitution of new materials in parts of existing design, frequently necessitating considerable costly trial and error experimentation on an actual production basis. When, at the beginning of World War II, it became apparent that mass production methods of forming would be required in the aircraft industry if the large numbers of military aircraft needed were to be supplied, renewed attention was focussed on the problem of sheet metal formability. It was widely recognized that the formability requirements placed on sheet metals had been steadily increasing in severity through the years, especially as greater and greater emphasis was placed on streamlined designs with the resultant freer application of doubly curved surfaces. The recent advent of several new high strength aluminum alloys of more limited formability than some of the older alloys also served to emphasize the need for new approaches to the problem. It seemed evident that progress in the technology of sheet metal forming would depend to a great extent on the development of more reliable criteria for the evaluation of formability. Although the problem is admittedly very complex, the most logical approach appeared to be through studies of the fundamental material properties of sheet metals, especially under complex stress conditions simulating those prevailing in actual forming operations. Most previous investigations have failed to make full use of existing knowledge of fundamental material properties, and in many instances have attempted correlations with properties which are now recognized as being ambiguous in nature. This investigation was undertaken, therefore, with the aim of developing methods for the study of the flow and fracture of sheet metals under combined stresses, and of making use of such methods as might be developed in

Jan 1, 1947

By E. A. Holbrook

The art of ore dressing is as old as civilization itself. Jason's search for the golden fleece was perhaps only the use of sheepskins for catching gold from gold-bearing sands washed over them. From Hoover's translation of Agricola we gather that in the middle ages ore dressing had advanced through the stage of hand sorting to water concentration by jigging. German methods and apparatus continued in the lead until the closing years of the past century; indeed, it is little more than a generation ago that many ore-dressing plants in this country were designed and operated by German-trained ore-dressing specialists. Meanwhile the development of the ore deposits in this country during the nineteenth century brought forth new inventions and methods. Blake's invention of the rock breaker in 1858 and the coming of the Wilfley table about 1896 are random examples of the improvements caused by our expanding needs. Yet ore dressing remained an art developed and practiced more or less by cut and try methods. The publication of the volumes on Ore Dressing by Dr. Robert H. Richards in 1903 marks the beginning of American ore-dressing practice as a science. Previously we had as guides only a few incomplete books based on foreign practice, or scattered references and articles in our own Transactions. Dr. Richards set down all the developments that had gone before, and outlined the ways for a scientific approach to the subject. He gave us a starting point. Since then ore-dressing practice and technique in this country have set the pace for the world. Coal preparation has been called "ore dressing upside down,'' because in ore dressing we generally save a small percentage of the heavy valuable mineral and discard the lighter gangue, whereas in coal preparation we save the larger quantity of light mineral and discard the smaller percentage of heavy waste. By comparison with ore dressing the history of coal preparation is brief, extending backwards hardly 100 years, for although coal had been dug and used locally for centuries it became an important article of commerce only with the coming of the industrial revolution 150 years ago. In new mines it was to he expected that the thickest and purest seams should be worked first. So long as these lasted there was little thought of coal preparation other than hand picking of the larger impurities and simple sizing to supply the real or fancied need

Jan 1, 1934

By Walter R. Hibbard

THE increased strength of a polycrystal-line metallic aggregate compared with that of its individual crystals generally has been associated with complex stress distributions at the grain boundaries resulting from atomic irregularity between grains. This disregistry, together with the necessity for adjacent crystals to deform 'compatibly regardless of the single crystal crystallographic strain mechanism, complicates this mechanism so as to increase the metal's resistance to deformation. Although Taylor1 has shown from purely mechanical considerations the requirement for at least five active slip systems to absorb the complexities during the homogeneous deformation of polycrystalline face-centered cubic metals, experimental studies by Barrett and Levenson2 indicate that this is feasible only in a qualitative sense because of deviations from homogeneous deformation. Seitz and Read in their review3 state: "Unfortunately . . . present knowledge of the grain boundary influence is not sufficient to complement the work in single crystals and provide us with a good foundation for treating polycrystals." The purpose of this investigation was to attempt to clarify the gap between single crystals and crystalline aggregates by an analysis of the effects of deformational stresses. Some of the results were described by C. H. Mathewson in his 1943 Campbell Memorial Lecture.21 PREVIOUS INVESTIGATIONS Since the performance of single crystals deformed under pure stresses has been relatively thoroughly investigated, the most significant researches are concerned primarily with deviations from single crystal behavior of large grained specimens. Qualitative grain boundary effects involving the observed amount of slip were reported by Carpenter and Elam5 in 1921. Individual crystals in a two or three grained aluminum specimen deformed by tension acted in the normal manner described by Taylor and Elam4 except for marked modifications at the grain boundaries. There the power to withstand deformation was considerably increased, leaving a ridge on the specimen where decreased slip occurred, often noticeable 34 in: from the boundary. Adcock,6 Yamaguchi,7 Seumel,8 Hirst9 and others have also reported this phenomenon as a qualitative trend. Yet attempts by O'Neill10 and Ljunggren11 to measure a difference in hardness at grain boundaries in undeformed specimens were unsuccessful. Miller12 measured quantitatively the reduction in slip near the boundary between the single crystal and polycrystalline areas of zinc specimens. These effects consisted of two parts: I. Next to the polycrystalline interface the distribution of stresses was so altered

Jan 1, 1948