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By J. R. Lucas, H. E. Rutherford

The primary objective of this research was to evaluate the feasibility of ultrasonic testing for the purpose of analyzing the structure and properties of rock material. A secondary objective of this study was to determine experimentally the elastic wnstants of various rock specimens with the use of ultrasonic equipment. Elastic constants can definitely be determined quickly and accurately by ultrasonic investigation. With proper equipment there are indications that ultrasonic waves could be utilized in the detection of flaws, such as fractures and planes of weakness, measurement of thickness, and the study of structure of rock material. Ultrasonic principles have been applied in many industries for the purpose of determining the structural characteristics of various materials. The principal applications of interest here are detecting flaws, measuring thicknesses, and determining elastic constants. The main advantage of ultrasonic analysis is that it is nondestructive. It also has extreme sensitivity, high penetrability, good accuracy, rapid response, and the necessity to have access to only one side of the specimen. These various applications and advantages lead one to think that ultrasonic principles might be applied to rock material in situ for purposes of analyzing its structural characteristics. Therefore, the primary objective of this research was to evaluate the feasibility of ultrasonic testing for the purpose of analyzing the structure and properties of rock material. A secondary objective of this research was to determine experimentally the elastic constants of various rock specimens with the use of ultrasonic equipment. The term ultrasonics is given to that branch of acoustics dealing with periodic sounds whose fre- quencies are above the audible range or above approximately 15,.000 to 20,000 cps. The first practical production of this high frequency sound was made possible after World War I due to developments of electronically controlled sound wave sources. At the present, the maximum practically attainable ultrasonic frequency is approximately 1000 megacycles per sec. Sound waves of sufficiently high frequency can be made to travel in a beam with little spreading. Therefore, such a beam can explore a material and detect nonhomogeneities in it by reflection. This is the principle of the ultrasonic reflectoscope invented by F. A. Firestone' in 1942. An ultrasonic beam, on pulse-penetratink a solid material medium, produces an echo when it strikes a flaw which has different acoustical properties than the surrounding medium. This echo can be detected by the same transducer which sends out the original pulse. This principle is the basis of the important industrial techniques of nondestructive ultrasonic testing of metals and other solid material. Later developments in the field of ultrasonic testing of solid material have been mostly improvements in equipment and instrumentation. To date, most of the industrial applications of ultrasonic analysis of solid bodies have been in the aircraft, electrical, and nuclear energy fields on the nondestructive testing of metal. The one solid material similar somewhat to rock material, upon which some work has been done to apply ultrasonic testing techniques to study structural integrity, is concrete. Jones and Gatfield3 briefly summarize this work on concrete. Their basic conclusion was that the strength of concrete was a function of the change of the longitudinal sound wave velocity in the concrete. Only recently has any extensive study been made to apply ultrasonic testing techniques to rock material. Lutsch studied rock material by an ultrasonic pulse method to determine the extent and degree of fracture of rock faces. Lutsch states that the number of observed reflections is a measure of the degree of fracture and that only ultrasonic waves are able to detect fractured zones subjected to high pressure. Suzuki, Sasaki, and Siohara5 studied the characteristics of the sonic wave in rock for propagation over a wide range of wave lengths. They indicated that, in rock, the propagation constant and attenuation of the

Jan 1, 1962

By Wallace W. Wilson

The Cook Ranch Field produces from a very permeable lens of Cook Sand of lower Permian or upper Pennsylvanian age, occurring at an average depth of 1.300 ft. The field was discovered in 1926, and has been operated with low pressure gas injection since July, 1927, one of the first such projects in Texas. Cumulative recovery to Dec. 31. 1950, was 14,701,131 bbl of crude oil, an average of 1,013 bbl per acre-ft of oil rection. and 72.5 per cent of the oil originally in place. Analysis of the reservoir performance indicates that grav-ity drainage has been an important factor in the producing mechanism. The high permeability and uniformity of the reservoir were extremely Favorable tor this type of operation. INTRODUCTION The Cook Ranch Field is the largest of a number of relatively small, shallow producing areas near .Albany, in Shackelford County, Texas. This field is one of the first to be operated by gas injection in Texas, and probably is the most successful low pressure gas injection project ever attempted. The field is owned entirely by Koeser and Pendleton, Inc., and Continental Oil Co., and has been operated by Roeser and Pendleton, Inc., since it was discovered. This study has been made possible through the cooperation of Roeser and Pendleton, Inc.. in making availahle a remarkably complete set of records covering all phases of their operations. The purpose of this paper is to present a summary of the history of the operations through Dec. 31, 1950, and to analyze some of the factors which appear to be responsible for the success of the project. Information concerning the physical plant and the early gas injection history has been presented in an earlier paper.' RESERVOIR CHARACTERISTICS production in the Cook Ranch Field is from a large lens of Cook Sand. of lower Permian or upper Pennsylvanian age, occurring at an average depth of 1.300 ft. The average dip of the sand body, as shown in Fig. 1. is only about 50 ft per mile to the northwest. The reservoir has an area of 930 acres and contains 15,512 acre-ft of Sand, consisting of about 14.512 acre-ft of produc-tive oil zone. and an estimated 1.000 acre-ft of primary gas-cap. The iso-pachous map (Fig. 2) was prepared from drillers' logs. Recent coring in the field has proven these logs to be quite accurate. The productive limits of the field are defined by shale on all sides but the southwest where a small zone of edgewater was encountered. This water does not appear to have encroached into the reservoir, and water production has been small. A smaller producing area to the south of the Cook Ranch Field also produces from the Cook Sand. but is separated from the reservoir under consideration by a band of shale. The sand consists of well sorted, coarse grained. rounded and subangu-lar quartz fragments. very poorly cemented. The analysis of 46 chip-core samples from two recently completed test wells indicates a range of porosity values between 12.5 and 28.2 per cent. wit11 an arithmetic average of 24.0 per cent. Air permeability values range between 50 and 2,300 md, with an arithmetic average of 1.200 md. The reservoir where cored is a Solid sand body. with no discernible major shale breaks or impermeable streaks. Vertical permeability appears to be of the same magnitude as the horizontal permeability. A core of the Cook Sand was cut ill the smaller field to the south, using lubricating oil as drilling fluid. The connate water content of the sand in this core was found to average about ten per cent, and the porosity and permeability were comparable with the values reported above. No analysis was made of subsurface or recombined hydrocarbon samples,

Jan 1, 1952

By G. A. Vissac

The only fine coal washer with proved automatic controls, the feldspar jig is capable of good efficiencies even at low separating gravities, handles a variety of products, and treats 150 tph and over. IN continental Europe the feldspar jig is used almost exclusively for cleaning the fine sizes of coal; it operates with an artificial bed, made up generally of pieces of feldspar or of any other hard and heavy rock with good cleavages. A primitive form of this machine requiring close supervision was used in this country years ago, but output was small. The modern machines are generally air-pulsated Baum-type jigs, with capacities up to 150 tph, and treat sizes from % in. to 0, usually previously dedusted or deslimed. These jigs are equipped with very accurate and sensitive automatic controls insuring satisfactory operation even at low separating gravity and with feeds irregular in quality and quantity. This paper will deal more particularly with coal cleaning separation, but the technical studies apply equally to all minerals. Theory of the Feldspar Jig To understand fully the operation of the feldspar jig and to appreciate its potential value, it is necessary to measure and analyze the motion of small particles of various specific gravities, falling in various media, under various conditions. As no practical formulas were available for that purpose, the writer has developed new theories and established new sets of formulas, which cannot be demonstrated here. They are applicable to all minerals and to many problems of coal or mineral concentration. These formulas do not pretend to absolute accuracy, but results, tested by comparison with experimentally recorded data, are sufficient for practical purposes, as they give definite indications of trends, relative values, and order of magnitude of the many factors involved. For pulsating motions no earlier formulas are available. In the case of continuous currents or motions, such formulas as Rittinger's, Allen's, or Stokes', over a hundred years old, apply only to special shapes and sizes of particles, involve factors and coefficients difficult to measure or appreciate, and deal only with free motions. They are of little use in solving practical problems. Units used with the formulas presented here are in the CGS system. Lateral friction and suction have been taken into account according- to methods currently used in aerodynamics, and only hindered motion is dealt with. As the feldspar jig is primarily intended to create a fluid bed condition, the mixture of fluids and solids obtained is homogeneous, and the apparent specific gravity of the separating medium is calculated accordingly. For instance, if 20 pct of the volume is coal and shale, with an average of 1.60 sp gr, in a liquid of 1.10 sp gr, the actual specific gravity of the separating fluid is 0.80 x 1.1 + 0.20 X 1.6 = 1.20. The fundamental equations are as follows: The general motion of a particle falling in a medium of specific gravity equal to u, hindered motion. is dv/dt = g/Ls [ L (s-u) - u/g v2 [1] g = 981 cm per sec, acceleration of gravity, and L = thickness of the particle of specific gravity (s) and velocity (v). The initial acceleration dv/dt = g (1-u/s ) [2] is a function of the specific gravity of the particle, only for a given medium, and independent of its dimensions—an ideal separating condition. The terminal velocity Vt = gxL- (s-u)/u, [3] for a given value of u, is a function of s and L. Two particles, L, s, and L2 s2, are said to be equivalent if they have the same terminal velocity, and accordingly L1/L2=s2-u/s1-u. [4] Two such particles cannot be separated by continuous currents, in any concentrating device. Because the initial accelerated motion, which provides for efficient separation, is followed by a constant velocity, which has a limiting effect, it is essen-

Jan 1, 1956

By J. E. Kirby, L. B. Schnitz, H. E. Stamm III

The production history of a gas-cap-drive reservoir was reproduced by calculations, and predictions were made for operations under primary depletion, pressure maintenance by gas injection, and pressure maintenance by water injection. Although the general equations used in this analysis have been available to the industry for a number of years, the procedure has not had extensive use because of the unusually large time requirements for developing numerical results. The use of digital computing equipment for processing the calculation work generally reduced the time usually required for an extensive analysis of this type. Calculation techniques were developed that were equally applicable for solving the gar-cap-drive problem, whether digital computing equipment or desk calculators are used. These techniques are outlined and the procedures are illustrated by the field problem. INTRODUCTION The analysis of a gas-cap-drive res-ervoir requires the simultaneous solution of the volumetric balance1 and displacement2 equations. Equations for the analysis of combination drive reservoirs were presented by Wooddy and Moscrip in a previous paper." These equations permit the evaluation of possible operating processes in order that the optimum method of pro- ducing the reservoir may be determined. Although these equations represent the basic technique known for the detailed analysis of gas-capdrive reservoirs, the calculation processes are quite complex and time consuming; hence, the procedure has not had extensive use. Recently, these equations were satisfactorily applied with the aid of a digital computer to investigate the completion history of a gas-cap-drive reservoir under the following operating methods: primary depletion, depletion under full pressure maintenance by gas injection, and depletion under full pressure maintenance by water injection. The use of digital computing equipment substantially reduced the time necessary for making the computations and permitted a more concise investigation of the reservoir's depletion history than was possible when the desk calculator was used. This more rigorous investigation also permitted a detailed analysis of the calculation procedures necessary in the solution of the gas-cap-drive problem. This paper outlines the procedure of analyzing a gas-cap-drive reservoir and illustrates the process with an actual field problem. CHARACTERISTICS OF THE RESERVOIR ANALYZED Production in the field under consideration is obtained from a Frio formation of Oligocene age at a depth of approximately 5,740 ft sub-sea. The accumulation, which is bounded on the flanks by strand lines, is semirectangular in shape with gentle narrowing toward the base of the structure as shown by the sand limits and completion map in Fig. 1. The reservoir development indicates an oil column of 319 ft that is defined by gas-oil and oil-water contacts. Basic data relative to the characteristics of the formation and the formation fluids are shown in Table 1. The formation exhibits considerable shaliaess and thinning near the oil-water contact indicating that little or no benefit will be received from natural water influx. This is substantiated by the fact that wells completed near the original oil-water contact have not produced water. A sizeable gas cap is present; however, considerable faulting is in evidence, and it is believed that only a limited portion of the gas cap will aid in oil displacement and pressure maintenance. Although the reservoir was in an initial stage of depletion, it was believed that as soon as the equilibrium gas saturation in the oil zone was exceeded and a number of upstructure wells were invaded by the expanding gas cap, the resulting high gas-oil ratio production would rapidly dissipate the natural drive and lead to limited oil recoveries and inefficient reservoir operation. This analysis evaluated the effectiveness of the primary displacement mechanism and

Jan 1, 1958

By D. C. Hilty, W. Crafts

A qualitative pseudoternary solidification diagram for the Fe-S-O system modified by manganese is proposed and supported by experimental derivation of an isothermal section at 1475°C and substantially 1 pct Mn in the solid-metal phase. The solubility of oxygen in liquid iron containing 1 pct Mn and sulphur contents up to 0.9 pct has been measured at 1600°C and found to increase as the sulphur content exceeds 0.15 pct. AS has been pointed out previously,' all oxide and sulphide inclusions in steel, excluding mechanically entrained matter, result from modifications of the basic Fe-S-O system. Therefore, one method of attack on the problem of the mechanism of deoxida-tion and inclusion formation is to examine the influence of deoxidizers on the Fe-S-O liquidus diagram. This approach has been adopted in work on the subject being carried out at the Metals Research Laboratories of the Electro Metallurgical Co. and has resulted in the postulation of types of solidification diagrams for the Fe-S-O system modified with common deoxidizers. This method has been of considerable assistance in interpretation of the factors affecting the formation of inclusions.' For the most part, however, these diagrams have been highly speculative. They were constructed primarily by inference from the pertinent binary and ternary systems and from the appearance of inclusions produced by specific deoxidizers. Moreover, since the systems contain four or more components, simplifying assumptions and qualifications were necessary in order to permit their representation as modifications of the Fe-S-O diagram. Consequently, experimental confirmation of the type of construction employed for these diagrams is desirable, and the present paper is concerned with such evidence. The addition of manganese to the Fe-S-O system was selected for initial investigation. Manganese is an important component of practically all steel and is, therefore, of fundamental interest. Because of its great affinity for sulphur, manganese has a more profound effect on the sulphide side of the Fe-S-O diagram than any of the other common deoxidizing eletments. In addition, more quantitative information pertaining to the contiguous binary and ternary systems involving iron, manganese, sulphur, and oxygen is available than for the other deoxidizers. Fe(Mn)-S-O Solidification Diagram Many of the side diagrams of interest in connection with this system are known. The Fe-Mn binary has been well established by several investigators;% the Fe-O system has been clarified by Darken and Gurry;' and FeO-MnO diagrams have been published by Herty,5 Andrew, Maddocks, and Howat,6 and by Hay, Howat, and White.7 The Mn-O diagram does not appear to have been derived experimentally, but the portion of 'it that is of interest can be visualized easily from a consideration of the melting points of Mn and MnO and the fact that a broad miscibility gap must exist between them. The ternary Fe-Mn-O diagram has been discussed by Benedicks and Löfquist,8 Wentrup,9 and by Körber and Oelsen.10 Experimental study of the Fe-Mn-O system has been carried out by Körber and Oelsen and to a lesser degree by Chipman, Gero, and Winkler,11 Hilty and Crafts," and others. On the basis of published information, then, an outline of the Fe-Mn-O liquidus diagram can be constructed as illustrated by Fig. 1. In this, as in all succeeding diagrams, transformations such as the ?-? reaction in iron have been ignored for purposes of simplification. The arrows denote falling temperature. The distinguishing feature of this diagram is the broad region of liquid immiscibility extending

Jan 1, 1955

By D. L. Harris

Chemical upgrading testwork on Stillwater chomite concentrate shows that reduction roasting and leaching (sulfuric acid and/or ferric sulfate) can provide upgraded feed to ferrochromium furnaces for making upgraded ferrochromium. Two-stage reduction smelting in electric arc furnaces can make upgraded ferrochromium also. Sulfating roasts and leaching (acid and/or water) results using gaseous SO2—SO3 or solid ammonium sulfate were not satisfactory for upgrading chromite. Chemical upgrading of domestic Stillwater (Montana) chromite has been considered at various times1'2' to provide a material with higher chromium to iron ratio, more like foreign high grade ore, for the production of standard grade ferrochromium. Physical bene-ficiation of Stillwater chromite ore can provide a ratio, Cr/Fe, no higher than the ratio in the chromite mineral, which is approximately 1.7. For comparison the analyses of a foreign metallurgical grade chromite ore, a high grade electrostatic process Stillwater concentrate and a stockpile concentrate from the Stillwater ore are noted in Table I. Single stage smelting of the high grade foreign ore with a ratio, Cr/Fe, of 3.37 can provide a ferrochromium of over 65 pct chromium content. Similar smelting of the Stillwater concentrate with a ratio of 1.7 can provide a ferrochromium of 50 to 55 pct chromium content.' It has been demonstrated on a pilot plant scale that chemically upgraded Stillwater chromite having a ratio, Cr/Fe, of 3.0 also can be smelted to provide a ferrochromium containing over 65 pct chromium.5 Two major considerations for an upgrading process are the ratio, Cr/Fe, in the product and the chromium recovery. A minimum ratio, Cr/Fe, of 3.0 is required in the product but for economic reasons a higher ratio is desirable for blending purposes as long as the recovery is satisfactory. Data from different kinds of chemical upgrading testwork are presented in this report. Some of the testwork was conducted to make a product which was not intended to be feed for ferrochrome smelting, but the data are considered pertinent to chemical upgrading. Results reported by others are noted also for comparison. WORK REPORTED BY OTHERS The U. S. Bureau of Mines has contributed much to the literature on chemical upgrading of chromite and a summary is given in Table 11. Reduction roasting and acid leaching were reported by Boericke and Bangert,1 by Lloyd and Gorst, et a1,2 and by Boericke3 to demonstrate very good success on a laboratory scale and only fair success in pilot plant tests for Stillwater (Benbow) concentrates. This work included basic studies on thermodynamic properties to explain the reduction and leaching results. Canadian workers, Downes and Morgan,9 have reported experimental success in upgrading a low grade Bird River chromite, similar to Stillwater material by the same process. Russian workers1' have noted results on reduction tests of high grade chromite which may apply to low grade ores and which help in understanding the reduction process. The use of flux additives in the reduction process was an innovation of their work. The Canadian workers9 also reported other kinds of experiments, including autoclave leaching of the chromite in a limited amount of sulfuric acid. An insoluble basic chromium sulfate was formed and separated from soluble iron, magnesium, and aluminum sulfates to provide an upgraded material. U.S. Bureau of Mines workers, Lloyd, Rosenbzum, Home and Davis,' reported on autoclave leaching of Benbow concentrates as a means of obtaining chromium alum for electrolysis. This last work required selective crystallization of alum to separate iron from chromium. Chloridizing roasting of Benbow and Mouat concentrates has been reported by Hunter and Banning6 and others8 to show that the iron chloride could be volatilized from the chromite to provide upgraded residues.

Jan 1, 1964

By E. A. Gulbransen, K. F. Andrew

THIS paper. will present the results of our studies on the kinetics of the gas phase reactions of co-lumbium and tantalum with O2, N2 and H2. Studies on zirconium and titanium have been previously reported.9,11 Due to their high melting points and their many excellent physical and chemical properties, colurn-bium and tantalum have been finding their places as useful metals in science and industry. Chemically the metals are very inert to gas and liquid phase corrosion at room temperature. However, at moderate temperatures of 250°C and higher the metals react readily with oxygen and hydrogen. It is of interest to study the gas phase reactions of these metals for the following reasons: (1) to compare the rates of the several reactions with those of other metals and to correlate the rate data with theory and structure predictions, (2) to add basic information on the practical difficulties of the reduction, refining and working of columbium and tantalum, (3) to anticipate new uses for the metals and (4) to understand the role that the metals play as components in high temperature alloys. Literature Survey A number of papers exist in the literature on the gas phase reactions of columbium and tantalum with O2, N2 and H2; however, only fragmentary data have been reported on the kinetics of these reactions. Although the free energy of formation of the oxide Ta2O520at 25°C has been determined and some thermodynamic work has been reported on columbium and its oxides, the data are not sufficient to make equilibria calculations at elevated temperatures. Oxidation: 1. Kinetics: The rate of oxidation of columbium and tantalum has been studied by McAdam and Geil23 using the interference color method. Tantalum is reported to oxidize more slowly than columbium, zirconium and iron. The amounts of oxidation of columbium after 20 hr in air for several temperatures are reported by the Fansteel Metallurgical Corporation.36 Columbium starts to oxidize in air at about 200°C. The oxide is said to be adherent and prevents further oxidation until the temperature is raised. Columbium is reported not to become brittle on heating in air for short periods like tantalum because the oxide film prevents further reaction. The columbium oxides dissolve into the metal when heated in a vacuum at temperatures between red heat and 1200°C. Above 1200°C the oxides are reported to evaporate. Columbium, in the oxide free state, is an active getter in vacuum tubes. 2. Preparation and Structure: G. Grube, O. Kuba-schewski and K. Zwiauer15 have studied the decomposition of Cb2O5 in argon. They find that CbO2 is formed slowly at 1150° and rapidly at 1300°C. Cb2O5 can be reduced to CbO2 by moist H2. The reduction of this dioxide to the lower oxides is rapid. By varying conditions CbO2, Cb2O3, CbO and Cb2O can be formed. CbO2, CbO and Cb2O have independent lattices while Cb2O3 is a stoichiometric mixture of CbO and CbO2. In a later paper O. Kuba-schewski" has shown that CbO is cubic and that CbO2 has a rutile type of lattice. The most exhaustive work on the oxides of columbium is that of G. Brauer.8 The number and constitution of the solid phases in the binary system Cb-O were investigated by the preparative, analytical and X ray methods. He indicates that only the oxides Cb2O5, CbO2 and CbO exist with limited regions of homogeneity. The solid oxide Cb,O, exists

Jan 1, 1951

By C. Bezemer, I. Havenaar

An investigation was carried out on the dynamic liltration behavior of drilling fluids. In a set-up consisting of a porous pipe through which the drilling mud was circulated, dynamic liltration rates and cake thicknesses were determined as a function of flow rate and filtration time. Eventually, a state of equilibrium was reached; i.e., both cake thickness and filtration rate attained constant values. Concurrently, dynamic filtration tests were carried out in a simple dynamic filter apparatus where mud flow was similar to that in a rotational vismmeter. In both arrangements the relation between equilibrium liltration data and rate of shear at the cake surlace was studied. Filter pipe and dynamic filter apparatus were lound to give identical relations. It was therelore concluded that the latter apparatus, which is suitable lor routine measurements on small amounts of mud, could be used to determine the dynamic liltration behavior of mud under borehole flow conditions. Some data are presented on the effect of filtration pressure and temperature on equilibrium filtration rate and cake thickness. INTRODUCTION In oil well drilling, the drilling fluid used generally forms a mud cake on the permeable sections of the borehole wall while filtrate is lost into the formation. As to the conditions under which this filtration process takes place, a distinction should be made between static mud filtration (mud is not circulating) and dynamic mud filtration (mud is circulating). In recent years several investigatorsl-5 have studied the process of dynamic mud filtration about which little had previously been known. This type of filtration is the subject of this paper which confirms several findings of previous investigators. It differs from already published works, however, in the following respects. 1. It contains a description of a simple laboratory apparatus developed for dynamic filtration measurements on small amounts of mud. 2. The effect of rate of shear at the cake surface on dynamic filtration has been studied. As a result of this study, dynamic filtration data pertaining to the borehole conditions of mud flow can be found from laboratory tests. 3. Some data are presented on the effect of filtration pressure and temperature on dynamic filtration. The work was limited to a small number of muds. No attempt was made to compare data on API filtrare loss with dynamic filtration rates. Previous workers have clearly shown that no correlation exists between static and dynamic filtration rates. EXPERIMENTAL ARRANGEMENT To establish whether the effect of mud flow conditions on dynamic filtrations is governed by the rate of shear at the cake surface, two different types of mud flow were used. In this connection the experiments were partially conducted by means of a porous pipe through which mud was circulated, partly in a dynamic filter apparatus which somewhat resembles a rotational viscometer. In both cases the flow conditions of the mud were well defined, thus making it possible to-calculate rates of shear at the cake surface. The filter pipe was 200 cm long with an internal diameter of 3 cm. Its perforated wall was covered on the inside with filter cloth on which the mud cake could form. Mud was pumped through the pipe at linear rates varying from 20 to 186 cm/sec. The required filtration pressure was obtained by means of a lack-pressure valve downstream of the filter pipe. In this arrangement the type of flow existing in the borehole is reasonably well simulated. The dynamic filter apparatus (Figs. I. and 2) consists mainly of two concentric cylinders with a clearance of about 0.5 cm. The outer cylinder (rotor) can be rotated at rates up to 1,000 rpm. The outer surface of the inner cylinder (radius about 2.5 cm) is covered with filter cloth or paper supported by copper gauze. The two cylinders are mounted inside a pressure

Jan 1, 1967

By Charles Stein

The effects of several different prior treatments an the creep behavior of 99.9995 pct aluminum at 260°C and 1000 psi canstant stress are compared with annealed specimens. Quenching from 538oC, irradiation with 2 mev electrons, and tension-compression room temperature fatigue damage were used to change the substructure of the specimens prior to their creep testing. The quenched and the irradiated specimens showed a larger primary and transient stage contribution to the creep curve than those specimens which were only annealed prim to creep testing. The specimen receiving prior fatigue damage at room temperature showed no first stage or transient creep when tested under identical conditions as the above specimens and had an average creep rate seven orders of magnitude lower than that of either the annealed, the quenched or the irradiated creep specimens. In a previous electron transmission microscopy investigationl of the substructure developed during the creep of pure aluminum at 0.57 Tm, it was noted that a large concentration of vacancy loops and dislocation loops were present in and near the subboundaries while the interior of the subgrains contained few of these defects and had a low dislocation density, see Fig. 1. Yim and Grant2 and Hazlett3 have shown that the presence in nickel of a substructure developed by prior cold work effectively reduces the primary and transient contributions to the creep curve. Hultgren,4 McLean,5 Gervais, Norton, and Grant,6 Chang and Grant,7 and others have shown the same effect with the higher stacking fault energy material, aluminum. However, the specific defect responsible for the change in the creep behavior developed by the prior cold work was not established. Specifically, what effectively interfered with dislocation motion in these materials at elevated temperatures? Was it jogs on dislocations produced by their interaction with other dislocations or with vacancy or dipole loops, see Fig. 1, or did the subgrain walls determine the mean free path for glissile dislocations? This would be a realistic possibility only if subgrain boundaries are effective barriers to dislocation motion. The ability of a subgrain boundary to act effectively against glissile dislocations depends on the number and the arrangement of dislocations in the subboundary,8 which in turn is a function of the creep strain.' This paper compares the creep rate of specimens possessing a large vacancy concentration to that of annealed specimens and with specimens having a stable subboundary wall containing Lomer locks produced by prior fatigue damage. EXPERIMENTAL PROCEDURE Vacancy Loops. Aluminum creep specimens, 99.9995 pct pure, were machined from zone refined rod to a 2-in. gage length and a cross-sectional area of 0.025 in. These specimens were annealed at 538oC, 1000°F, for 10 min and quenched into ice water. They were then reheated to the creep test temperature of 260°C, 500°F, and held at this temperature for 18 min to al-low for vacancy condensation and loop formation. The specimens were subsequently creep tested at 1000 psi constant stress at 260°C. The temperature along the gage length was monitored by three Pt-Pt, 13 pct Rh thermocouples, two embedded in the upper and lower shoulders of the specimen and one attached to the mid-point of the gage length- The temperature gradient was held to ± l°C or less throughout the Creep test. Elongations were measured by two LVDT's 'connected in an averaging 'On-figuration, with quartz extension arms placed against the specimen at the extremes of the 2-in. gage length. i K 3J?--' * *H - >^> - ' ^L r 77 . *y J OJL, J Fig. 1—Transmission electron micrograph of pure aluminum strained 8.2 pct at 260°C and 1000 psi constant stress. Note the presence of numerous loops near the light dislocation tangle

Jan 1, 1970

By O. K. Miniato, L. Massé, K. Nobe, J. S. Aronofsky, W. F. 213-000-000-016 Seyer

MUCH work has been done dealing with the effect of mechanical stress on electrode potential in an electrochemical system. The contradictory nature of the experimental results indicates the complexity of the problem although thermodynamic considerations show that a simple relationshir, should exist. In those systems where a gas was the electromotive active substance satisfactory agreement between theory and practice has been found. Des Coudres' found this to be so even when the active substance of the electrode, in this case mercury, was in the liquid state. In contrast, attempts to correlate theory and experiment for the solid state have met with a very limited success. The early workers in this field, Andrews,2 Walker and Dill3 used iron, certainly one of the most reactive of metals. Others have made use of less active metals such as copper and nickel. Recently Fryxell and Nachtrieb4 investigated the electrochemical behavior of gold and silver under both tensile and compressive stresses and concluded that it was doubtful whether true stress potentials could ever be measured. Much of the lack of success to measure the thermodynamic stress potential can be ascribed to the presence or formation of a complex film on the metal surface in contact with the electrolyte. Further, the theoretical stress potential is very small and therefore difficult to measure directly. Thus the calculated emf between a 24 B & S gage cold-drawn copper wire stressed with a weight of 1 kg and an unstressed portion of the same wire is only 2.60 X 10"7 volts. This is very small compared to that which can be produced by chemical reactions at the metal electrolyte interface which in turn can be so large as to mask completely the stress potential. Hence in this type of measurement all chemical side effects must be eliminated or reduced as much as possible. It was for this reason that the system copper-sodium chloride solution was selected for study. INSTRUMENTATION In the many preliminary experiments conducted, two major difficulties were encountered. The first was to measure the small electro-potentials to be expected and the second to obtain a suitable electrode surface. The conventional potentiometric method was found to be unsatisfactory for measuring the small emf expected. However, by using an L & N No. 2290 galvanometer having a resistance of 915 ohms consistent measurements were possible. The reference electrode was always the unstressed one made from the same sample of wire. The steady current flow was approximately 10-8 amp. Lewis and Randell5 have stated that for currents of the order of 10-8, if there is no sensible polarization, the measured emf may be taken as a reversible one. To check the galvanomenter readings an alternative method was devised to measure the potential difference between the wires. This involved a Liston-Falb d-c breaker amplifier model 10, an L & N k-2 potentiometer and a moving-coil galvanometer having a sensitivity greater than 0.1 µv (microvolt) per mm. To increase further the output voltage of the amplifier a d-c amplifier, model B. L.-932 was introduced into the circuit. This amplifier was in turn connected to a Brush recorder which had been calibrated previously by the test signals from the Liston-Falb instrument. These test voltages employed took into account the impedance of the input current. Unfortunately, this method had too low a sensitivity for measurement below 10 µv. Above this value the voltage agreed reasonably well with those obtained directly by the simple galvanometer method. The main advantage of the amplifier setup was that one did not have to wait until no deflection occurred on the galvanometer in the circuit when first exposing the wires to the solu-

Jan 1, 1959

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

The effects of increasing hydrogen content, introducing a notch, and changing the strain rate on properties of titanium and one of its alloys were investigated over a range of testing temperatures from —196° to 200°C. Both high purity and commercial purity A-55 titanium were used as representative a materials, while a commercial Ti-8 pct Mn alloy was used for an a-P alloy. It was found possible to analyze the data, using the ductile-to-brittle transition temperature concept. Increasing hydrogen, the presence of a notch, and increasing the testing speed raised the transition temperature for the a materials. The presence of hydrogen and notches raised the transition temperature of the a-B alloy also. However, increasing the testing speed generally decreased the transition temperature of the a-p alloy. IN previous papers, the authors have shown that hydrogen is most detrimental to the notch-bend impact toughness of a-titanium' and to the tensile ductility of a-B titanium alloys.' These general effects have been confirmed by Kessler and co-workers," and by Kotfila and Erbin." Kessler showed that the slower strain rate in notch-rupture tests was a more sensitive measure of hydrogen embrittle-ment of a-B alloys than the tensile test. In the present paper the authors cover, with tensile and notch-bend tests, the effect of testing speed, notches, and testing temperature on hydrogen em-brittlement. High purity and commercial purity titanium, examples of u materials, and a commercial a-,f3 Ti-8 pct Mn alloy were investigated. The purpose of the investigation was to correlate the factors producing embrittlement. Materials The high purity titanium for this investigation was obtained by arc-melting crystal bar from Foote Mineral Co. into 1 Ib ingots. As-cast hardnesses for these ingots ranged from 60 to 90 Brinell. The arc-melted ingots were forged to % in. diam rods at 1470°F. These rods were swaged to & in. diam at room temperature prior to machining of the specimens for hydrogenation and testing. The commercial A-55 titanium and the Ti-8 pct Mn alloy were obtained from Rem-Cru Titanium Inc., as % in. diam rod. The A-55 titanium was hot swaged to 1/4 in. diam at 1300°F prior to machining of the specimens for hydrogenation and testing. The a-p C-11OM alloy was hydrogenated prior to hot swaging to 1/4 in. roc1 at 1300°F. Hydrogenation prior to fabrication permitted testing of the a-P alloy in the equilibrated and stabilized condition. The equilibration and stabilization treatment used was an air anneal for 1 hr at 1300°F, followed by furnace cooling to 1100°F and then air cooling. Hydrogenation was done in a Sieverts apparatus described previously.' The hydrogenation treatment consisted of heating for 1/4 to 1/2 hr at 820 °C in purified hydrogen, slow cooling to 680"C, holding 1 hr for homogenization, and rapid cooling to room temperature. Intended hydrogen levels for the a-tita-nium materials were 0.05, 0.5, 1.0, 1.5, and 2.0 atomic pct—about 15 to 430 ppm. For the Ti-8 pct Mn alloy, the intended hydrogen levels were 0.05, 0.5, 1.0, 2.5, and 5.0 atomic pct—about 15 to 1100 ppm. The material for the 0.5 atomic pct level of hydrogen was vacuum annealed prior to hydrogenation to increase the accuracy of the addition. Vacuum annealing to remove hydrogen consisted of heating for 6 hr at 820°C, and resulted in a hydrogen content of about 10 to 15 ppm. When hydrogen contents were above 0.5 atomic pct—100 ppm—the hydrogen was added without prior vacuum annealing.

Jan 1, 1957

By S. B. Twiss, P. R. Basford

The relationship between areas of iron powders, briquettes, and sintered compacts and tensile strength has been determined. It has been found necessary to distinguish between two types of areas which exist in such powders—a macroscopic area due to the shape and size of particles and a microscopic area due to pores and cracks in the surface. Only the macroscopic area, specifically the area due to particle irregularity, contributes to tensile strength; the microscopic area cannot be forced into contact with adjacent particles ond does not participate in bond formation. Of the two methods of area measurement employed in this study—permeability to liquids and gas-phase adsorption—only the former is useful for determining the roughness factor. A measure of this roughness, (area measured by permeability to liquid) -f- (orea of powder with the same size distribution, but made up of spherical particles), is shown to be uniquely related to tensile strength at constant density. The other important factors in determining the strength of sintered-metal compacts are the density and presence or absence of surface oxide. THE manufacture of metal parts by the process of powder metallurgy is an important and rapidly growing industry. Progress has been rapid and continuous, largely because of the excellent research in the field. Nevertheless, the process remains inherently complex and empirical. Several investigators have shown that the properties of the final compact must depend on many variables; namely, shape,' size distribution,"-" nd compositiona of the original particles, the pressure necessary to compress to the desired density, the density of the compact, the time and temperature of sintering, and so on. Through the application of some new techniques to the study of powders and compacts, and the correlation of a number of observations of known variables, the present paper attempts to clarify and simplify the underlying theory of the powder-metallurgy process. Any theory must start with the obvious fact that the strength of a compact, its most useful property, is due to the formation of welded areas between adjacent particles, and attempt to deduce what effect other variables will have on (a) the area and (b) the intrinsic strength of these welds. Such welded areas can be demonstrated by electron micrographs, as in Fig. 1. It was believed that (a) could be most directly studied by means of surface-area measurements on the original powders and on the compacts made from them; the area decrease should be related closely to the welded area. A representative group of eleven iron powders from commercial sources, and made by a variety of processes, was chosen for this study. In addition to the surface-area measurements, correlations were established between the tensile strength and all the known variables which might possibly affect it. The results are quite unexpected. They indicate that the situation is much simpler than the authors had anticipated. The strength of the sintered compact is determined, indeed, by no more than three variables; viz., the irregularity of the original particles, the density of the compact and, in exceptional cases, the amount of surface oxide. All three had been recognized previously as having some effect on the tensile strength, but in the absence of the special techniques and interpretations to be developed here, there could be no suspicion that they were the only relevant variables. Materials and Methods Material—All the iron powders were commercial products obtained from the Amplex Division of Chrysler Corporation. Powders A, B, C, and J were very pure electrolytic iron. Powder D was made from oxidized scrap reduced by heating with an excess of cast iron. Powder E was a high-grade iron ore reduced by hydrogen. Powder I was prepared by atomizing molten cast iron in an air blast, quenching the droplets in cold water, and crushing the coarse powder. Mill scale (oxide) is added and the mixture heated to reduce the high carbon content. The other powders were all prepared by reduction of iron oxides, such as mill scale. They

Jan 1, 1959

By William P. Blake

The frequent association of apatite in layers in the midst of magnetic iron-ore is highly significant of a stratified and organic origin of both minerals. Usually the phosphate of lirne is more abundant

Jan 1, 1893

By Stewart R. Wallace

"For his achievements in unravelling the complex geology of the Climax ore body; for his leadership in the discovery of the Henderson deposit; for his continued encouragement of young geologists; and for his lecture . .."

Jan 1, 1975

By H. Souder

The object of this paper is to bring to the notice of engineers a safety detonating fuse by the use of which misfires in blasting may be eliminated and safety in blasting operations promoted.

Jan 1, 1915

By Robert D. Pehlke, Arden L. Bement

A mass transfer coefficient for the removal of hydrogen from liquid aluminum by inert flush degassing has been determined experimentally at 700°C. A mathematical model has been derived, assuming transport control, which adequately describes the experimental data. The removal of hydrogen is shown to increase with decreasing bubble size, and with increasing flow of flushing gas. The presence of hydrogen in liquid metals in amounts which exceed the solid solubility at one atmosphere hydrogen pressure is highly undesirable, causing unsound ingots or castings, or resulting in difficulties during further fabrication. The removal of hydrogen from liquid metals can be accomplished by several methods, the principal two being vacuum treating and inert flush degassing. The design of a process involving either of these techniques is based on the mass transfer coefficient for hydrogen between the liquid metal and a hydrogen-dilute gas phase. In an effort to extend our knowledge in this area, an investigation of the rate of removal of hydrogen from liquid metals by inert gas flushing was undertaken. In view of the difficulties encountered with gas porosity in the casting of aluminum and aluminum alloys, and because of certain experimental advantages, liquid aluminum was selected for the study. PREVIOUS INVESTIGATIONS The removal of gases from liquid metals, particularly steel, has received considerable attention in recent years, The first definitive work of a theoretical nature was presented by Geller1 who considered the case where equilibrium exists between purging gases and metal bath during flushing, and also deviations from this ideal case. Hulme2 has surveyed a number of experimental studies and discussed some of the practical limitations of removing dissolved gases from molten metals. More recently a number of studies have been reported on degassing of steel melts by flushing with an inert gas.3'4 Considerable work has also been reported on aqueous and organic liquid-gas systems, and an excellent summary prepared by Hovis.5 The treatment of liquid aluminum by a flushing gas to remove dissolved hydrogen has been known for several decades.6 A number of gases have been used for this purpose, including nitrogen, argon, and chlorine, or mixtures of these gases. Tikkanen and Erkko7 have studied the relative density changes of aluminum castings poured from melts degassed with chlorine, nitrogen, and mixtures of the two gases. Their

Jan 1, 1962

By A. F. Taggart, Nathaniel Arbiter

The chemical reaction occurring in collection of nonmetallic minerals with amine-type collectors was early postulated by students of flotation phenomena to be metathesis between the mineral and the collector, involving exchange between the amine-bearing (aminium) ion and the cation of the mineral, and formation at the mineral surface of an oriented film of the amine salt of the mineral anion. Qualitative evidence of exchange has been obtained on several occasions at Columbia. Thus 1000 C.C. of a solution containing 495 mg of laurylamine hydrochloride was shaken 17 min. with 100 grams of barite and ground in a porcelain mill to pass a 200-mesh screen; the mixture was then set aside for 48 hr. Filtrate therefrom analyzed 476 mg. per liter of laurylamine hydrochloride. There was no substantial loss of chloride ion (78.4 mg. per liter in the original; 74 in the filtrate). No successful analyses were concluded for barium ion. Earlier, confessedly rough work with scheelite indicated a solution gain in Ca++ equivalent to about one-half the aminium ion lost. Real quantitative roof of the exchange, in the form of an established stoichiometric balance, is unknown to the authors. The data of the present paper, however, obtained from experiments designed on the basis of the exchange hypothesis, constitute strong evidence of its truth, and at the same time point the way to economic utilization of the expensive nitrogen-bearing collectors in concentration of the low-priced nonmetallic minerals. The basic postulate underlying the experiments performed was that, if the collecting reaction is of the type R+ + Y- + MX = RX + M+ + Y- where R = aminium ion, Y = the anion of the amine salt, and M and X are, respectively, the cation and anion of the mineral, the reaction should obey qualitatively the implications of the mass-action and solubility-product laws. This is to say that coating and collection should be aided by the addition to the solution of either ion (R+ or X-) of the collector-coating compound, and hindered by the addition of either of the ions M+ or y-. Experimental work comprised determination of (,) the relative solubilities of the laurylammonium salts of a variety of nonmetallic-mineral anions; and (21 the contact angles' of various minerals in solutions containing different concentrations of the postulated controlling ions. Semiquantitative flotation tests were run With barite as checks on the diagnostic character of the contact angles. The amine

Jan 1, 1947

By Bailey Willis

IN 1882, Peckham put forward a provisional hypothesis to account .or the distillation of petroleum.1 He did not formally state the hypothesis, but in a discussion of facts drawn from many fields he made it clear that he regarded petroleum, and especially the petroleum of the Pennsylvania fields, as a "fractional distillate produced under high pressure and consequently at a comparatively high temperature.?2 He quotes James Hall on the geology of the Appalachians and says:3 It is not necessary here to discuss the nature or origin of metamorphic action. It is sufficient for our purpose to know that from the upper Silurian to the close of the Carboniferous periods the currents of the primeval ocean were transporting sediments, sorting them into gravel, sand, and clay, forming gravel bars and great sand beds beneath the riffles and clay banks in still water, burying vast accumulations of sea weeds and sea animals far beneath the surface. The alteration, due to the combined action of heat, steam, and pressure, of the formations of the Appalachian system from Point Gaspe in Canada to Lookout mountain in Tennessee, involving the Carboniferous and earlier strata, distorting and folding them, and converting the coal into anthracite and the clays into schists along their eastern border, could not have ceased to act westward along an arbitrary line, but must have gradually died out farther and farther from the surface (source?). The great beds of shale and limestone containing fucoids, animal remains, and even indigenous petroleum must have been invaded by this heat action to a greater or less degree, and that "chronic evaporation" of Prof. Lesley must have been the inevitable consequence. From an investigation of the relations between coal and petroleum, White has" more recently concluded as follows: (1) Petroleum is a product generated in the course of the geodynamic alteration of deposits of organic debris of certain types buried in the sedimentary strata. (2) The quantity and characters of the oils generated are determined by: (a) the composition of the organic deposit at the beginning of its dynamo-chemical alteration; (b) by the stage in the progress of the dynamo-chemical alteration of the organic substances; (c) by the elimination, under certain conditions, of the heavier and more' viscous hydrocarbons through filtration incident to migration.

Jan 1, 1920

By Nathaniel Arbiter, A. F. Taggart

The chemical reaction occurring in collection of nonmetallic minerals with amine-type collectors was early postulated by students of flotation phenomena to be metathesis between the mineral and the collector, involving exchange between the amine-bearing (aminium) ion and the cation of the mineral, and formation at the mineral surface of an oriented film of the amine salt of the mineral anion. Qualitative evidence of exchange has been obtained on several occasions at Columbia. Thus 1000 C.C. of a solution containing 495 mg of laurylamine hydrochloride was shaken 17 min. with 100 grams of barite and ground in a porcelain mill to pass a 200-mesh screen; the mixture was then set aside for 48 hr. Filtrate therefrom analyzed 476 mg. per liter of laurylamine hydrochloride. There was no substantial loss of chloride ion (78.4 mg. per liter in the original; 74 in the filtrate). No successful analyses were concluded for barium ion. Earlier, confessedly rough work with scheelite indicated a solution gain in Ca++ equivalent to about one-half the aminium ion lost. Real quantitative roof of the exchange, in the form of an established stoichiometric balance, is unknown to the authors. The data of the present paper, however, obtained from experiments designed on the basis of the exchange hypothesis, constitute strong evidence of its truth, and at the same time point the way to economic utilization of the expensive nitrogen-bearing collectors in concentration of the low-priced nonmetallic minerals. The basic postulate underlying the experiments performed was that, if the collecting reaction is of the type R+ + Y- + MX = RX + M+ + Y- where R = aminium ion, Y = the anion of the amine salt, and M and X are, respectively, the cation and anion of the mineral, the reaction should obey qualitatively the implications of the mass-action and solubility-product laws. This is to say that coating and collection should be aided by the addition to the solution of either ion (R+ or X-) of the collector-coating compound, and hindered by the addition of either of the ions M+ or y-. Experimental work comprised determination of (,) the relative solubilities of the laurylammonium salts of a variety of nonmetallic-mineral anions; and (21 the contact angles' of various minerals in solutions containing different concentrations of the postulated controlling ions. Semiquantitative flotation tests were run With barite as checks on the diagnostic character of the contact angles. The amine

Jan 1, 1947

By W. A. Backofen

THE preferred orientations, or textures, resulting from many of the various methods for testing and forming metals have been the subject of numerous investigations.1,2* Despite this large amount of work, however, only a few limited studies have been made of the texture that is developed by torsional deformation. Ono3 found that in severely twisted wires of copper and aluminum a [Ill] direction lies parallel and a [1101 direction perpendicular to the longitudinal axis of the wire. Sachs and Schiebold4 have reported that a double-fiber texture exists in a twisted aluminum wire with both the [Ill] and [loo] directions parallel to the axis of the wire. Twisted iron wires have also been examined by Ono.8 Both the [1101 and [1121 directions were reported as parallel to the axis of the wire. Goss5 concluded from a study of twisted rods of a low-carbon steel that the preferred orientation existing at fracture is quite complex, but that many grains have a [1101 direction parallel to the axis of the wire. In addition to the earlier experimental work, some suggestions have been made about the possible nature of the torsion texture. These suggestions are based on the results of many experiments which indicate that the cold-working texture of a particular metal is largely determined by the geometrical change in shape that the metal undergoes during plastic deformation.1,6 Hibbard and Yen7 have considered the problem of deformation textures and have presented an analysis which is able to explain why equivalent changes in shape should yield similar textures. Therefore, a knowledge of the principal strains associated with torsional deformation would seem helpful in the interpretation of the torsion texture. The necessary analysis has been made of the state of strain in an element of metal lying in the surface of a cylindrical rod or tube that has been subjected to pure torsion.8,9 This analysis shows that the directions of the principal normal strains rotate continuously within a torsion specimen while it is being twisted. After the first infinitesimal amount of twisting, these directions make angles of 45" with the longitudinal axis of the bar. They rotate from this position as twisting proceeds, and after an infinite amount of twisting, the direction of the principal tensile strain is perpendicular, and the direction

Jan 1, 1951