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By D. S. Tomalin, D. F. Stein

The effect of reducing oxygen to low concentrations on the fracture of high-purity iron single crystals has been examined at 78° and 20°K. It is found that iron single crystals grown by the strain-anneal method usually contain a few occluded grain boundaries which may become embittled in the presence of oxygen, thereby nucleating cleavage fractures. High purity with respect to interstitial elements was found to inhibit twinning and evidence is presented for an orientation dependence of the resolved yield stress. Deformation occurred by slip rather than twinning at both temperatures of testing with elongations of as much as 9 pct at 20°K. THE fracture properties of iron single crystals have been observedl-3 to be a function of temperature, orientation, and purity. Allen, Hopkins, and McLennan1 demonstrated that at 78°K iron single crystals became increasingly brittle as the tensile axis approached the (001) pole of the stereographic unit triangle. Iron crystals with the tension axis near a (001) pole were completely brittle and orientations near the (011)-(111) boundary were very ductile, achieving a 100 pct reduction in area prior to fracture. Later work of Biggs and pratt2 and of Edmondson3 demonstrated that by reducing the carbon content of the single crystals the transition between brittle and ductile failure at 78°K could be shifted to orientations nearer the (001) pole. Ed-mondson went further and pointed out that any mechanism which tended to increase the yield strength of the iron (i.e., carbon addition, pre-strain) also increased the tendency for brittle behavior at 78°K. Thus by a reduction of carbon content Biggs and Pratt were able to obtain ductile behavior to within 20 deg of the (001) pole, and Ed-mondson was able to obtain ductile behavior to within 26 deg of the (001) pole. Edmondson's material had a total interstitial content (carbon, oxygen, and nitrogen) of approximately 60 ppm and, although Biggs and Pratt reported no analysis, indications were that their iron contained comparable impurities. Stein, Low, and seybolt4 purified iron single crystals to a total carbon, oxygen, and nitrogen content of approximately 20 ppm. They observed a lowering of the yield stress with this increased purity, and thus one might have expected an observation of increased ductility. Although they tested specimens of orientations which the previous workers had indicated should be ductile, the crystals failed at a 78°K in a brittle manner with little elongation. Stein noted,' however, that about 90 pet of the failures could be traced in origin to occluded grains. Allen et al.1 and Edmondson3 do not report examination of their cleavage surfaces, but Biggs and pratt2 reported that microscopic examination of the cleavage surfaces of many of their specimens revealed the presence of small occluded grains. Honda and cohen6 and Keh7 have also observed the initiation of fracture at occluded grains in iron single crystals. Therefore, the additional complication of occluded grains must be considered in studying the properties of iron single crystals and the origin of fractures determined if the ductility exhibited by the crystals is to be considered meaningful. Various investigators8-12 have studied the effects of impurities on grain boundaries in high-purity polycrystalline iron. Rees and Hopkins10 showed that the addition of oxygen to low-carbon (0.002 pet) iron weakened the grain boundaries, causing a shift from transcrystalline to intercrystalline fracture and a progressive decrease on the brittle-fracture stress with increasing oxygen content. In addition, it has been shown by Low and Feustel11 that the addition of carbon to polycrystalline iron containing oxygen eliminated grain boundary brittleness. Thus, oxygen can embrittle grain boundaries in high-purity polycrystalline iron, but the addition of an appropriate amount of carbon can eliminate the oxygen-induced brittleness. The oxygen content (19 ppm) of the iron "single crystals" employed by Stein el al. was large enough to suspect impurity effects at the occluded grain boundaries. Allen et al.1 Biggs and pratt,2 and Edmondson3 may have masked any occluded grain problem in their specimens considering the relatively high carbon levels they employed. stein13 demonstrated that the addition of as little as 0.9 ppm C to previously purified (less than 5 x 10-3 ppm C) "single crystals" would increase the elongation from a few percent to more than 20 pet at 78°K and the fracture was not associated with grade boundary initiation.

Jan 1, 1965

By John H. Hall

The Frémont test for measuring the energy consumed in breaking a notched bar of steel is not so well known in this country as it deserves to be. The test specimen used in this test is about # by 6 by about 16 in., notched with a hack saw on the lower side to cause the piece to break at a fixed point. A weight of 10 kg. falling 4 m., and provided with a knife or chisel which strikes the specimen, breaks the test piece by impact. The residual force in the falling weight after it has broken the specimen is recorded by a suitable device, and the difference between the total energy and the residual energy of the weight (in kilogrammeters) is the force consumed in breaking the specimen. An experience of several years with the Frémont testing machine has shown its great value in readily detecting brittleness not revealed by tensile testing or slow bending testing. In this paper it is proposed to discuss (1) the supersensitiveness of the test as applied to cast steel and (2) its value in revealing the effect of heat treatment under certain conditions. In testing coupons cut from castings heat treated by quenching and annealing, attention was drawn to the wide variations in the value of the Frémont test of specimens cut from different parts of the coupon. The latter was of the form and dimensions shown in Fig. 1, and Fremont test pieces were cut from two parts of this coupon, marked A and B in that figure. The results of the tests are shown below, tests A and B in each instance being from the same coupon: A. B. A. B. Coupon. Kilogram- Kilogram- Coupon. Kilogram- Kilogram- meters. meters. meters. meters. 1,........ 12.0 12.5 9,........ 27.5 32.5 2,........ 11.0 32.5 10,........17.5 31.0 3,........ 11.5 30.0 11,........ 14.5 31.0 4,........ 20.0 33.0 12,........ 15.0 27.5 5,........ 17.5 33.0 13,........ 19.0 30.0 6,........ 17.5 20.0 14,........ 17.5 25.5 7,........ 17.5 13.0 15,........15.0 30.0 8,........ 10.0 30.0

Jan 1, 1914

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 E. R. Parker, R. H. Thielemann

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By R. H. Thielemann, E. R. Parker

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The microhardness of single crystals of tungsten disilicide has been investigated by the Knoop method. The average random room-temperature hardness of the WSi, matrix was 1350 kg per sq mm. Hardness crnisotropy was noted with respect to plane and indenter orientation as determined by single-crq.stal X-rny studies. Annealing at 1600" and 1800°C decreased the average hardness to 1310 and 1230 kg per sq tnm, respectively, and produced a second phase identified by X-ray diffraction and electron-microprobe analysis to be wSio.7. Ball-impact experiwzents produced rosettes at 850°C. Optical and electron microscopy showed evidence of slip and cross slip and twinning produced by microhardness indentations. Prismatic (100), [001] slip was found and cor~elated with hardness data. THE present study was undertaken to investigate the hardness anisotropy of as-grown and annealed single crystals of tungsten disilicide. The existence of the silicide WSiz in the W-Si system has been well-established and its structure thoroughly investigated zachariasen2 found WSi, to have a tetragonal C type of structure, similar to that of MoSi, with lattice parameters a = 3.212A, Kieffer et al. studied the W-Si system and measured the density and microhardness (at a 100-g load) of both polycrystalline WSi, and WSi,.,. The values found were 9.25 g per cu cm and 1090 kg per sq mm for WSi,, and 12.21 per cu cm and 770 kg per sq mm for WSi0.7, respectively. According to Samsonov et a1.5 the microhardness of polycrystalline WSi2 is 1430 kg per sq mm (at a 120-g load). EXPERIMENTAL The WSi, single-crystal boules investigated in this paper were grown by a Verneuil-type process using an electric arc by the Linde Division of the Union Carbide Corp.6 The largest specimens were 8 mm in diameter by 16 mm long. The crystals had an average density of 9.01 g per cu cm with a tungsten • silicon content of 99.9 wt pct. The major impurities were: 87 ppm O, 41 ppm N. 54 pprn C, 500 ppm Zr, 50 ppm Na, and 50 ppm Mn. The crystals were silicon-poor, the average silicon content being 22.20 pct (stoichiometric value is 23.40 pct), and tungsten-rich, the average tungsten content being 77.70 pct (stoichiometric value is 76.60 pct). As-received single crystals were ground and analyzed by powder X-ray diffraction technique using Cu Ka radiation. Laue and layer line rotation patterns were obtained on cleaved sections of WSi, single crystals. Electron-microprobe traverses of representative crystals were done using a Phillips-AMR electron microanalyzer. Carbon replicas were used to prepare electron micrographs. This work was done with a JEM-6A electron microscope. Prior to the metallographic examination, the specimens were mounted in Lucite and then polished for short times on polishing wheels using 9-, 3-, and 1-p diamond-grade pastes. Finally they were fine-polished with Linde A powder for 24 hr on a Syntron vibratory polisher. The samples were etched with 4H 2 O:1HF:2HNO3, which is a medium fast-acting etchant. The combination 1HF:2HNO3:5 lactic acid is also a satisfactory etchant. Annealing runs for selected specimens were made at 1600" and 1800°C for 3 hr at 1.0 to 3.0 x 10-5 mm Hg. A Brew tantalum resistance furnace with WSi2 powder for setters was used. The WSi2 powder was the same as that used for the crystal growth. Temperatures were measured with a calibrated W, W-26 pct Re thermocouple and a microoptical pyrometer. Powder X-ray diffraction, emission spectrographic, and electron-microprobe analyses were done after the annealing runs. For microhardness measurements a Tukon Microhardness Tester Type FB with a Knoop indenter was used. Although measurements were taken at loads ranging from 25 to 1000 g, the 100-g load was chosen as the standard load. All measurements were taken at room temperature. Only indentations of cracking classes 1 and 2 were considered.' DISCUSSION OF RESULTS Powder X-ray diffraction analysis showed the as-received crystals to be single-phase WSi2. Laue and layer line rotation patterns obtained on cleaved sections of WSi2 single crystals proved them to be tetragonal WS 2 2 The results also indicated that the c axis of the crystal was oriented parallel to the boule or growth axis. Electron-microprobe traverses across the matrix of the as-grown crystals showed them to be homogeneous WSi,. Optical and electron microscopy of etched crystals, however, revealed that they contained minute amounts of the "golden" and the "blue" second phases as opposed to the "white" or WSi2 phase. These two second phases were concentrated in inclusion and etch-pit

Jan 1, 1965

Jan 1, 1955

By Oliver S. North

Reserves of perlite rock in the western section of the United States are immense. A geological report prepared for the Union Pacific RR showed proved tonnage of over 400 million tons in southern Nevada alone. Yet the perlite industry is not large, and most of the mines are relatively small. There are indications that perlite processing, thus far largely in the hands of relatively small com¬panies, is becoming concentrated in a few large companies. For economic reasons the bulk of perlite sold in crude form has come from three or four pro¬ducers, although many individual operators have sold small quantities to limited lists of purchasers. Perlite is one of ultra-lightweight aggregates. Owing to its outstanding qualities as an aggregate, variety of uses, and ultimate economy of use, it has enjoyed considerable popularity in this country in recent years. Marked foreign interest also has been evinced in this material.

Jan 2, 1955

By Ed Van Eeckhout

As part of a U.S. Bureau of Mines-sponsored project on the utilization of "stiff" backfill to minimize potential rock burst hazards, a finite element study was undertaken to predict stresses and displacements around a stope mined up from the 5400 level of the Sunshine mine, Kellogg, Idaho. This stope was to be backfilled using a high-modulus fill. In preparation for that configuration, certain instrumentation was installed near the 5400 level to monitor stress changes. Due to untenable economics, only 2 cuts of the stope were ever made. This paper presents the results of the instrument readings taken during the first cut and compares them with the numerical predictions, as well as presents the modeling results of closure and fill stresses in the stope if it had been mined.

Jan 1, 1984

By J. A. Rowland, C. W. Funk

THIS investigation is a part of the United States Bureau of Mines work in conserving the Nation's resources. The isothermal sections presented were developed as a guide to a comprehensive investigation of the properties and fabricating characteristics of copper-base alloys containing manganese and tin. These alloys are being investigated as possible replacements for the commercial bronzes containing substantial quantities of tin. Development of the isothermal sections has, therefore, been limited to the area between 0 to 20 pct Mn and 0 to 25 pct Sn. Since Heusler1 reported the ferromagnetic properties of the Cu-Mn-Sn alloys in 1903, the system has been the subject of several investigations. These studies were largely concerned with correlation of magnetic properties and crystal structure.2-6 Vero,' however, established the solidus surface of the system, between 20 pct Mn and 40 pct Sn, by thermal and microscopic methods. The a, ß, and y solid solutions were also observed by Vero and reported to extend into the interior of the ternary system. For the present study, the annotated diagram of the Cu-Sn system prepared by Raynor' and the Cu-Mn diagram by Dean and coworkers9 were used as the binary borders of the ternary system. Procedure The metals used in this investigation were electrolytic manganese, washed cathode copper, and three-star tin. The manganese, produced at the Boulder City pilot plant of the Bureau of Mines, had a purity of 99.9 pct; the copper contained less than 0.004 pct Bi and 0.001 pct S; the tin contained 0.070 pct Pb, 0.070 pct Sb, 0.050 pct Fe, and 0.065 pct Si. Heats of 1 lb were melted in alundum crucibles with a 3-kw induction furnace. The heats were chill-cast in iron or copper molds to form 6-in. ingots 3/4 in. in diameter. Molds were washed with graphite or zirconia, depending on the manganese content, and preheated to 150°C. The maximum impurity content of any alloy was 0.03 pct Fe, 0.02 pct Si, and 0.02 pct Al; in most cases, they contained less than half this quantity of any of these impurities. Composition of the alloys and their treatment prior to homogenizing are shown in Fig. 1. Designations adjacent to each composition refer to the heat numbers. With a few exceptions, ingots containing 20 pct Sn or less were hot-swaged. These ingots were swaged, after a 24-hr preheat at 650°C, to obtain a total reduction of 70 pct in cross section. Intermittent reheating was necessary, and reductions were limited to either 0.025 or 0.050 in. in diameter per pass. Selection of a 200-hr homogenizing treatment was based on extensive experiments which indicated that virtual equilibrium was reached after 150 hr. Structures were retained by quenching in water. Grain sizes in the specimens homogenized at 350" and 450°C were generally small. These homogenizing treatments were preceded by a 50-hr anneal at 650°C to facilitate phase identification by increasing the grain size in these specimens. The specimens were furnace-cooled from this temperature to the homogenizing temperature, and the heat treatment was continued for the standard 200-hr period. The homogenized samples were bisected to provide an internal section for metallographic examination. Optimum definition of the microstructure was obtained by successive polishing and etching. Quarter-strength ASTM copper reagent No. 13 gave the most satisfactory results.10 Filings from interior sections of the samples were used for diffraction studies. These filings were annealed in evacuated glass tubes at homogenizing temperatures for periods exceeding 50 hr and quenched in water. During this treatment the manganese content was reduced by significant amounts, probably by vaporization. This change in composition was considered in applying the diffraction data, which were used only as a means of identifying phases where the data were consistent with the metallographic evidence. Phase Identification The a solid solution is readily distinguished by the copper-colored, twinned, polyhedral grains, as shown in Fig. 2, and a face-centered cubic X-ray pattern. Tukon indentations, using a 25-g load, indicate a Knoop hardness of 155 for a quenched from 650°C. Using white light developed by a Wratten 78 A filter, the ß grains in etched specimens have a dark brown tint in contrast to the lighter copper-colored grains of the a phase. Knoop hardness values of 284 were obtained for the ß structure in specimens quenched from 650°C. The ß structure was also distinguished from the a phase by its body-centered cubic lattice. The acicular structure appearing in Fig. 3 was evident in several alloys of higher tin content after quenching from either 750' or 650°C. Since a trans-

Jan 1, 1954

By Robert A. Rapp, Ronald L. Pastorek

Solid-state electrochemical measurements by three alternative experimental procedures were made with the cell FeO, Fe3O4 |Zro.85Cao.15O1.85 |Cu| Zr0.85CaO.15O1.85 | FeO, Fe304 to establish the solubility and diffusivity of oxygen in solid copper in the temperature range 800" to 1030°C. The solubility of oxygen in solid copper and the diflusivity of oxygen in solid copper Dgu = 1.7 X 10-2 exp(-16,000/RT) Cm2/sec were determined and confirmed in alternative experiments. The enthalpy of solution of oxygen in solid copper equals —10,000 cal per mole; the partial excess entropy of the oxygen atoms in the Cu-O dilute solution is approximately the same as that found for interstitial atoms in other metals. The diffusivity of oxygen in solid copper is consistent with that expected for an interstitial atom. RELIABLE values for the saturation solubility N(s) and diffusivity DO of oxygen in solid copper have not been unambiguously established in the literature. Following three early determinations by others,1"3 Rhines and Mathewson4 reported that the solubility of oxygen in solid copper increased from 0.007 at. pct 0 at 600°C to about 0.015 pct at 1050°C. Phillips and skinner,, using essentiially the same analytical procedure, reported that the solid solubility increases from 0.0018 at. pct 0 at 550°C to about 0.0075 pct at 1050OC. The only previous value for the diffusivity of oxygen in solid copper was reported by Ransley.6 Ransley deoxidized Cu-Cu2O alloys in an atmosphere of carbon monoxide gas to yield a solubility-diffusivity product. He used the solubility data of Rhines and Mathewson to calculate the diffusivity values. Another method for obtaining the solubility-diffusivity product (N(s) DO) is by measuring the widths of internal-oxidation zones in copper alloys as reported by Verfurth and Rapp.7 However, the calculated N(S)Do products depend upon the alloy content of the specimen, so that the internal oxidation of copper alloys does not follow ideal internal oxidation kinetics. As a result, unequivocal values for the N(s) DO product were not obtained by this procedure. A solid-state coulometric titration technique similar to that employed in this work was introduced by C. Wagner8 to study the dependence on silver activity of the Ag/S ratio in silver sulfide in the temperature range of 160" to 300°C. Similar experiments have been carried out by C. Wagner and co-workers9-11 to study the stoichiometry range of silver and copper tellurides, cuprous sulfide, and cuprous selenide. Numerous authors have carried out electrochemical measurements with a solid oxygen-ion-conducting electrolyte to determine the solubility and/or diffusivity of dissolved oxygen in several liquid metals.12-l6 Rickert and Steiner17,18 have used solid-state electrochemical measurements to determine the diffusivity of oxygen in solid silver from 760" to 900°C. Two different cell geometries were used. In the cell of linear geometry Fe, FeO | ZrO2 + (CaO) | Ag + [0 (dissolved)] [1] oxygen diffused from the interior of the silver electrode to the silver/electrolyte interface where the oxygen activity had been lowered from a fixed initial value to practically zero by the application of voltage to the cell. The diffusivity of oxygen in solid silver was determined from the solution of the diffusion equation and the time dependence of the cell current. However, this determination of the diffusion coefficient depended upon a knowledge of the solubility of oxygen in solid silver. A cylindrical geometry was used for the cell Pt, O2(Po2 = 0.21 atm) | ZrO2 + (CaO) | Ag + [0 (dissolved)] [II] which also allowed the diffusivity of oxygen in solid silver to be determined. These values were in agreement with other available data.l9 Recently, Raleigh20,21 used a method involving the measurement of diffusion-limited currents in a cell involving the AgBr solid electrolyte to determine the diffusion coefficient of silver in Ag-Au alloys at 400°C. Diffusivity values on the order of l0-14 sq cm per sec were measured in the alloy composition range 10 to 60 at. pct Ag in a single experiment. From numerous electrical conductivity and galvanic cell measurements,9'22"26 the solid solution Zr0.85 Ca0.15 O1.85 has been established as an electrolyte with predominant oxygen ion conduction over a wide range of intermediate and high oxygen activities. For interrelating the thermodynamics and the kinetics of the dissolution of oxygen in solid copper in this investigation, a galvanic cell was constructed with FeO-Fe3O4 as the reversible reference electrode, the Zr0.85Ca0.15 O1.85 electrolyte, and a pure copper specimen under-saturated in oxygen as the other electrode. THEORETICAL ANALYSIS Three variations of a high-temperature electrochemical technique were used in this study to provide two determinations each of the solubility and diffusivity

Jan 1, 1970

By R. H. Frazier, J. M. Hodge, F. W. Boulger

This paper reports the results of studies of the impact properties of quenched and tempered alloy-steel plates as a function of sulfur content. It was found that the impact energy levels decreased continuously as the sulfur content increased and that there was a straight-line relationship between impact energy and sulfur content when plotted on logarithmic coordinates. Cross rolling raised the level of these Lines for transverse tests and lowered the level for logitudinal tests proportionately to the amount of cross rolling. ALTHOUGH it has been generally recognized that, for applications in which notch toughness is critical, the sulfur content of the steels used should be held to a low value, quantitative information on the effect of sulfur on notch toughness has not been available. For such applications, it is a common practice to specify minimum impact values, and in order that these may be met consistently it is important that the steel producer know quantitatively the effect of sulfur on notch toughness so that realistic sulfur content limits can be applied to the steels they produce. In many instances, particularly in flat-rolled products, impact properties are specified in the direction transverse to the principal rolling direction, so that the factors affecting the anisotropy or directionality of impact properties are also of concern to the steel producer. For some applications, furthermore, it is a common practice to increase the sulfur content of steels in order to improve their machinability, and, in such instances, the effect of this practice on notch toughness may often be of concern. This paper reports on an investigation, carried out at Battelle Memorial Institute, designed to furnish this quantitative information on the effect of sulfur on notch toughness and also to furnish further information on the factors affecting the anisotropy of impact properties in wrought heat-treated alloy steels. MATERIALS AND EXPERIMENTAL PROCEDURE The experimental steels were of intended base analysis: 0.30 pct C, 0.80 pct Mn, 0.25 pct Si, 2.5 pct Ni, 0.80 pct Cr, and 0.45 pct Mo. Steels were made with sulfur contents varying from 0.005 to 0.179 pct. The steels were prepared from 600-lb induction-furnace melts. Steels containing 0.020 pct or more sulfur (at meltdown) were melted from a charge of ingot iron (except for one heat): lower-sulfur steels were made from electrolytic iron. The charge consisted of ingot or electrolytic iron, ferrosilicon to give 0.10 pct Si, and ferromanganese to give 0.05 pct Mn. At meltdown, electrolytic nickel, ferromolybdenum, iron phosphide, and pyrite were added followed in sequence by ferrochromium, sili-comanganese, ferrosilicon, and ferromanganese. The slag was then removed and graphite added to give the desired carbon content. Bath temperature was adjusted to 2850°F and, when no other additions were to follow, 2 lb per ton of aluminum was added, immediately before tapping. Compositions of the experimental steels appear in Table I. Analyses are from single determinations, except sulfur which was analyzed in duplicate. A test sample (3 in. in diam by 6 in. long) and a 575-1b ingot were poured from each heat. The test sample was poured in a sand mold; the cooling rates of the test sample and the large ingot were approximately the same. Chemical analysis chips and metal lographic specimens were taken from the test samples. The ingot was 8 in. sq at the base and 9 in. sq at the top. A 5 X 5 X 6-in. sand mold hot top was completely filled in teeming the ingot. After solidification, the mold was stripped from the ingot which cooled to room temperature. Ingots were reheated to 2250"F and rolled to 1.9-in. slabs on a commercial mill. The slabs were box-cooled to room temperature. Sections of the 1.9-in. slabs were heated to 2250°F and rolled on a Battelle laboratory mill according to one of three schedules: 1) rolled straightaway to 0.5-in. plate; 2) rolled straightaway to 1.3-in. thickness, then cross rolled to 0.5-in. plate (29 pct cross rolling); or 3) cross rolled from 1.9-in. to 0.5-in.-thick plate (46 pct cross rolling). The 0.5-in.-straight- or cross-rolled plates were normalized at 1700°F for 1 hr and then water quenched from 1600°F. Plates were then tempered 2 hr at 1240°, 1170°, 1080°, or 860°F to obtain Rockwell C hardness of 25, 30, 35, and 40, respectively. Tempering was followed by quenching to room temperature to avoid temper embrittlement. Slack-quenched plates were isothermally transformed for 26 min at 800°F, quenched, and tempered 2 hr at 1170°F. Pearlitic microstructures were obtained by holding 168 hr at 1200° F, followed by quenching. Charpy V-notch specimens were taken both transverse and longitudinal to the main rolling direction, notched perpendicular to the plate surface, and tested. Slabs and plates which were to be homogenized

Jan 1, 1960

By F. R. Brotzen, D. L. Davidson

ALTHOUGH much effort has been devoted to the problem, the nature of plastic flow in bcc metals is still not fully understood. Some of the difficulties encountered stem from the scarcity of information on orientation effects and the uncertainty as to the glide system in these metals. In an attempt to provide some of this information, the present investigation was carried out, using zone-refined molybdenum single crystals deformed in tension and in direct shear. Considerable evidence exists to indicate that the primary slip system for molybdenum is (110) <111>.1,2 Figs. 1 and 2 indicate that this is, indeed, the case for direct shear at room temperature (see Ref. 3 for a description of the shear-testing equipment and procedure). Moreover, from Fig. 2, the shear stress on the (123) is lower than that on the (112). This would be the case if, as has been suggested,4,5 slip on these two planes is in reality com-

Jan 1, 1965

By Arthur Phillips, C. H. Mathewson

During the past year considerable work dealing with the mechanical properties and microstructure following the anneal under uniform condi-tions of certain types of commercial rolled brass has been done in this laboratory. Since these experiments were conducted with the active cooperation of the Bridgeport Brass Co., involving free use of its product, and have thus furnished information which is characteristic of some of its special mixtures, full publication of the numerical relationships and comparative results encountered does not seem justifiable. Some of the more general features of this work are, however, available and it is our present purpose to use the material in question, along with some results of special tests, in discussing the characteristics of recrystallization as related to the degree of hardening by strain and the ordinary annealing variables. We desire to make acknowledgment of the many courtesies extended by Mr. Charles Ferry, Metallurgist of the Bridgeport Brass Co., and the value of his cooperation, which has greatly stimulated the study of brass in this laboratory. A clear and systematic presentation of the principal relations between temperature and time of anneal, the changing physical properties and microstructure and the degree of previous reduction by cold-rolling, was first made, in the case of rolled brass and copper, by the French engineer, C. Grard,&apos; in 1909, although much fragmentary information of this general character had appeared earlier and the main facts involved were undoubtedly known to many brass specialists through their own private research. From this work, it appears that in the cartridge mixture (67 per cent. copper, 33 per cent. zinc) the properties imparted by cold-working within the limits, 13 to 75 per cent, reduction of area by rolling Original Area — Final Area 0.13 to 0.75), are not affected by anneal- Original Area " ing for a 50-min. period at any temperature below 200°C. At or in the

Jan 1, 1916

By ALFREDO INTZAUGARAT, MIGUEL BERRO

During the years 1943 through 1945, there was a decrease in the total oil production in Argentina. In the fields of Comodoro Rivadavia (Chubut Territory) and Mendoza and Salta Provinces, the production obtained was as shown in Table I. The only place where there was a small increase was Plaza Huincul, in the Neuquen Territory and Lunlunta, in the Mendoza Province.

Jan 1, 1946

By George W. Riter

OUR mineral-land laws need revising so as to provide definite title at the outset to the mineral deposits within any definite piece of land. The laws as they now stand, especially those applicable to lodes, breed uncertainty as to rights of possession prior to patent; and to my mind this is the worst feature of all, worse even than the apex bugbear. It is now almost impossible for anybody to tell-with certainty what mineral rights exist within any area that is not covered by patent, or whether any valid rights exist at all. Our system is unique in permitting individuals to appropriate and exploit mineral lands of the public domain without notice of any kind to the Federal government, and to relinquish them without any ceremony at all. The result is a clouded record that cannot be cleared up until each claimant is put to some sort of final proof. In order to accomplish this, new Federal legislation will be required. The requirements for a mineral survey and the proceedings for patent have always been cumbersome and expensive; and perhaps out of regard for the poor claim owner, who can ill afford the outlay for that sort of thing, the law does not require him to go. through it unless he chooses to do so. Consequently, every active mining district has become encumbered with tangled groups of doubtful or conflicting locations, whose rights and boundaries, when any valuable ore is found, must usually be determined by lawsuits that are as expensive and as distressing as the stakes are high. So deeply has litigation entered into our mining system that a claim whose rights have never been disputed would probably be set down offhand, by $miner of the old school, as of no value. Think of the litigation over rights of possession on the Com-stock lode—12 leading companies involved &apos;in an aggregate of 245 suits within a period of less than eight years! Ambiguous local records; the chance of erroneously placed or obliterated monuments; doubt as to the sufficient performance of the statutory annual labor; uncertainty as to prior conflicting or overlapping locations; anxiety as to the changing attitude of the Department of the Interior and the Forest Service—such considerations as these make an unpatented mining claim an unclean thing in the eyes of possible investors. Is it any wonder that they keep themselvesand their money at a safe distance,

Jan 1, 1915

By A. L., Bailey

All who are even generally aware of the tremendous rate of increase in coal washing operations must realize the growing importance of the float-and-sink test. I believe it is conservative to estimate that, in the past decade, the dollar volume of float-and-sink testing has increased tenfold. It is a simple matter of economy, then, to examine the factors that determine the cost of adequate float-and-sink testing. When the Coal Preparation Section of the Bureau of Mines entered upon a greatly expanded program of such work in connection with the synthetic liquid fuels investigations, it seemed advisable to examine these factors experimentally. The principal consideration that differentiates float-and-sink test sampling from general purpose sampling, is that the original particle size must be preserved. Therefore, the total cost of the test will be directly affected by any standard that might be proposed to limit sample bulk reduction at any given particle size. For this reason, the relationship of sample size to variability of results was the first factor to be studied experimentally.

Jan 1, 1949

New York Meets first Wednesday after first Tuesday of each month. DAVID H. BROWNE, Chairman. PERCY E. BARBOUR, Vice-Chairman. A. D. BEERS, Secretary, 55 Wall St., New York, N. Y. C. A. BOHN, Treasurer. Boston Meets first Monday of each winter month. W. E. C. EUSTIS, Chairman. - R. L. AGASSIZ, Vice-Chairman E. E. BUGBEE, Secretary-Treasurer, Mass. Inst. of Technology, Boston, Mass. ALBERT SAUVEUR, H. L. SMYTH. Columbia Holds four sessions during year. Annual meeting in September or October. STANLY A. EASTON, Chairman. FREDERIC KEFFER, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. D. C. LIVINGSTON. FRANK A. ROSS.

Jan 12, 1916

The General Electric Co., in cooperation with the Montana School of Mines and under a research grant from the Anaconda Co., is presently experimenting on a new non-explosive method of breaking rock with radio-frequency electrical power. The method is known as electrothermal forcing. It must be understood that present equipment has not been designed to perform primary blasting functions. Its conceived use will be restricted to small pieces of rock too large to pass through a chute or grizzly. However, even this use is still far in the future. Experiments to date have been limited mostly to rock smaller than 18 in.

Jan 11, 1961

THERE is at least one concrete indication that Soviet Russia&apos;s two most important iron ore producing centers are seriously depleted. While keeping in mind Russia&apos;s penchant for reverse propaganda, one piece of evidence indicates that Magnitugorsk in the southern Urals and Krivoi Rog in the Ukraine have been mined to a point where lower grade ores are being recovered. An article in Pravda, Soviet newspaper, by I. P. Bardin. a Russian metallurgist, says that ore presently mined must undergo an expensive enriching cycle before it can be used in blast furnaces. Com- pounding Russian metallurgical troubles is the low quality of coking coals. High ash and sulphur content typifies the coal Badin talks about. Coal from the Ukraine, Eastern Siberia, Kazakhstan, and the Far East requires extensive treatment before it can be used, according to the article in Pravda.

Jan 7, 1953