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By E. J. Ostrowski

The history of ironmaking dates back to 4000 BC when an open forge was used to produce a sponge iron from a heap of ore and charcoal. Even at this early date, man recognized the need for a fuel and a reducing agent. As time passed, man developed new methods of producing iron; however, these developments were centered on the mechanical aspects, and as a result, a furnace evolved which is now known as a blast furnace. During this period of evolution,' man struggled with the only fuel he knew - charcoal. Some 5600 years passed before any attempt was made to use coal as a fuel for the blast furnace. The use of coal had its beginning in 1619 when Dud Dudley of England first attempted its use in the blast furnace; as a-fuel and as a reducing agent. Coal charged to the top of the blast furnace was not satisfactory. The volatile matter of the coal choked the flues, and also the poor, strength qualities would not support the weight of the ore. Breaking up of the coal compacted the stock column to an impervious mass. One hundred and sixteen. years later in 1735, Abraham Darby of England introduced coke as the fuel and reducing agent in the blast furnace. The acceptance of coke as a fuel for the blast furnace was not spontaneous. As late as 1870, one-half of the pig iron product of the United States was made with anthracite coal, 30 per cent with raw bituminous coal and coke, and 20 per cent with charcoal. However, by 1910, 96.2 per cent of the blast furnace product was made with coke, 2.4 per cent with anthracite and coke admixture, and 1.4 per cent with charcoal. Coke became the standard fuel in the blast furnace. As the art of ironmaking progressed, more pig iron was produced and more coke was consumed. Coke oven capacity was progressively increased. In 1910, there existed approximately 4,000 coke ovens; in 1960 there was approximately 15,000 ovens. This increase in coke oven capacity was necessary to feed the mammoth appetite of modern blast furnaces.

Jan 1, 1962

By W. A. Backofen, F. de Kazinczy

FRACTURING under conditions of particular interest is identified with the junction of curves relating tensile yield and fracture stresses to test temperature; the intersection point gives the lowest stress, for brittle fracture (at the ductility transition temperature). An expression for is found in Cottrell's brittle-fracture analysis, Eq. [15],1 while measurements of this stress and temperature have been reported for a low-carbon steel heat treated to differ-

Jan 1, 1962

By R. S. Wagner, W. G. Pfann

METHODS that have been used to measure stress relaxation in metals and plastics have been reviewed recently by G. R. Gohn and A. FOX.' The ideal stress relaxation test comprises placing a sample under a constant strain (usually considered

Jan 1, 1962

By B. H. Kear

All the possible ways of forming simple two-dislocation boundaries in multiple slip orientations are deduced. It is shown that the principal differences in work hardening behavior of crystals plastically deformed in these orientations can he accounted for in terms of the likelihood of formation of diffuse boundaries, or deformation bands, consisting of the products of dislocation reactions of the Lomer type. Also, it is pointed out that the break-up of boundaries under the applied stress is more likely to yield interstitial jogs than vacancy jogs, whereas glide dislocations cutting throuqh dislocations trapped in particularly stable boundam'es can acquire both types of jogs. USING Frank's' grain boundary formula, Ball and Hirsch2 determined the parameters of all the possible boundaries that can be built from two sets of glide dislocations in the fee structure. This paper deduces the geometrical possibilities for the formation of these two-dislocation boundaries in the different multiple slip orientations, and discusses the role of boundaries in work hardening and in jog formation. Formation of Two-Dislocation Boundaries in Mutiple Slip Orientations. The parameters of the possible two-dislocation boundaries for any crystal orientation can be deduced most conveniently using the boundary formulae due to Amelinckx,3 in conjunction with the stereographic projection shown in Fig. 1. Suppose that slip occurs in a-BC and ß-CA. According to Amelinckx, when the two systems of glide dislocations are parallel, the rotation axis, u, of the boundary is parallel to (a x ß) and the unit normal, u, defining the boundary plane is parallel to (a x ß) x (BC x CA). On the other hand, when the glide dislocations form a crossed grid, u is parallel to (BC x CA) and u is parallel to (a x CA) x (ß x BC). In Fig. 1, (a x ß) is the pole of the great circle passing through a and ß, so that u is parallel to DC, i.e., parallel to [110]. Furthermore, (a x ß) x (BC x CA) is the pole of the great circle passing through DC and 6, so that u is parallel to [110]. Hence, when all the glide dislocations are parallel, the boundary is pure tilt with parameters u = [110], v = [ 110]. Similarly, it may be shown that the corresponding crossed grid of dislocations is a mixed boundary with u = [111], u = [111]. Consider the case of a crystal compressed in the [001] orientation. In this orientation, according to Fig. 1, there are eight available slip systems. In what follows, the different types of two-dislocation boundaries that are possible in this orientation will be examined by taking different combinations of two slip systems out of the available eight, with a-BC always one of the systems. Case (i)—Slip Systems a-BC and d-CB. The formation of a tilt boundary in (101), which consists of a crossed grid of edge dislocations with vectors BC andCB, is illustrated in Fig. 2(a). As the figure shows, slip is required in the system a-BC in one part of the crystal and in d-CB in the other part, with both sets of dislocations entering the boundary from opposite sides. The rotation axis of the boundary lies in (101), depending on the relative densities of the two sets of edge dislocations in the boundary. Case (ii)-Slip Systems a-BC and ß-CA. The two possible boundaries are shown in Figs. 2(b) and (c); boundary (b) is tilt with u = [110], u = [110], and

Jan 1, 1962

By Richard D. Graves

Pitch from low-temperature carbonization of bituminous coal was hydrogenated at cracking conditions in a continuous bench-scale unit to produce low-molecular-weight oils and tar acids. The pitch contained 15.6 pct benzene-insoluble material, 4.0 pct hexane-soluble oil, and 80.4 pct asphaltene by weight. At 475° C, 7,500 psig, and 1.5 hours residence time, hydrogenation products, based on the weight of pitch, were about 36 pct oil boiling below 325° C, 24 pct hexane-soluble heavy oil, 17 pct asphaltene, 1 pct benzene insolubles, and 12 pct hydrocarbon gases. The yield of tar acids boiling below 250° C was 4.3 pct, and the yields of C6 to C8 paraffins, naphthenes, and aromatics were each less than 1.0 pct. The yield of tar acids was within the range of yields obtained by hydrogenation or high-temperature carbonization of bituminous coal (2 to 5 wt pct). Yields of oil boiling below 325° C increased with increased residence time or temperature. There was little or no effect of residence time on yields of alkali- soluble material which contained tar acids. Yields of hydro-carbon gases increased markedly with an increase in temperature from 475° to 500° C. Lowering the hydrogen pressure to 4,500 psig resulted in yields similar to those obtained at 7,500 psig.

Jan 1, 1962

By J. H. Waxweiler, L. C. Ikenberry, R. J. Bendure

Carbon which is present as insoluble carbides in austenitic stainless steels can be measured quantitatively by dissolving the steel in iodine-methanol and analyzing the residue for carbon. Severe sen-sitization was observed in Type 302 due to precipitation of only 0.003 pet carbon. Both cold work and the presence of delta ferrite caused a marked acceleration in rate of carbide precipitation. Carbide precipitation rates in 17-7 PH were stzulied for the austenite conditioning and also the aging heat treatment. CARBON and its compounds exercise a major influence on the properties of stainless steels and their response to thermal treatment. Sensitization in 18-8 type stainless steels has been the subject of numerous investigations throughout the years. Bain, Aborn, and utherford," and Binder, Brown, Frankss all studied the effects of heating austenitic stainless steels in the temperature range of 1000° to 1500°F. The primary purpose of most of these studies was the investigation of susceptibility to in-tergranular attack in acids due to these sensitizing heat treatments. Intergranular precipitation of carbides was always associated with intergranular attack but it was recognized2 that severe attack could occur with but minute quantities of precipitated carbide. Mahla and ielsen utilized the electron microscope to make a significant contribution in illustrating the appearance and method of growth of chromium carbides during sensitizing heat treatments. However, as they stated, their studies of residues could not be used to obtain a quantitative measurement of the amount of carbon which was actually precipitated. The aim of the present investigation was to devise a relatively fast, simple method for the quantitative measurement of carbides in stainless steel. EXPERIMENTAL WORK The initial investigations were made to determine the best means of separating carbides from the matrix. A number of dissolving media were tried using both chemical and electrolytic attack. Qualitative examination of the extracted residues by X-ray diffraction indicated that solution in iodine-methanol would furnish a good means of separation. Consequently, further work was pursued along this line. The method is quite simple. The sample in the form of millings or nibblings is dissolved in iodine-methanol solution at room temperature (6-g iodine, 25-ml methanol per g of sample). The insoluble residue containing the carbides is separated by suction filtration through an ultra-fine glass filter disc. This is a very fine filter medium that will retain particles as small as 0.1 to 0.2 p in diameter. After washing with methanol and drying, the filter disc and residue are placed in a conventional combustion carbon-tube furnace and the carbon determined gravimetrically. Using this technique it was found that reproducible insoluble carbon values were obtained. However, since such small amounts of insoluble carbon were obtained on Type 302 after sensitizatipn at 1250°F and 1500°F, the values were confirmed by a second method. In the second method the sample was dissolved with copper potassium chloride and filtered through a millipore paper. This treatment dissolves the matrix but leaves undissolved practically all of the carbon irrespective of how it is present in the steel. The amount of insoluble carbon present as chromium carbide is determined by calculation from the analysis of the residue for chromium and iron. The derivation of the formula used for this calculation is discussed later. The values obtained by the indirect copper-potassium-chloride method were in agreement with those obtained by the iodine-methano1 method. See Table I. It should be pointed out that the sensitivity of the direct combustion method is not too high when the amount of carbide present is small. This is due primarily to inherent blanks and to analytical errors such as weighing. For this reason it cannot be stated with any degree of certainty that there is a significant difference between values of 0.002 and 0.005 pct. Having confirmed that the iodine-methanol extraction gave a quantitative measurement of the precipitated carbides in Type 302, exploratory tests were conducted on Armco 17-7 PH stainless steel. Samples from commercial Heat 54807 were solution annealed at 2000°F, water quenched and heated at 1250" and 1500°F, and water quenched. The analysis of Heat 54808 is as follows:

Jan 1, 1962

By J. N. Ong

The oxidation of tantalum is assumed to occur by four simultaneous first-order chain reactions; solution of oxygen in the metal, nucleation and growth of a suboxide phase at the metal surface and two phase boundary processes which give rise to two different modifications of Ta2O5. A rate equation is then formulated which accounts for all principal details of oxidation behavior, unifies and correlatss the results of the principal investigations, and expresses the rate as a function of pressure, temperature, and time. For purposes of practical application, the expressions: may be used below and above 700T respectively to determine the regression rate of tantalum in cm per hr, where T is to be expressed in "K and P in atmospheres pressure of oxygm. The equations will reproduce within a factor of two all reported experimental rates in the temperature range 475" to 1400°C and pressure range 0.000026 to 40.8 atm 0. 1 HE oxidation kinetics of tantalum have been investigated thoroughly in the temperature range 50" to 1400 and pressure range 1.32 x l0-' to 40.8 atm pressure of 0,and as a result, the principal features of the oxidation of tantalum are known and have been described in considerable detail. The exposition of the characteristics of the behavior of tantalum in oxygen has been largely descriptive, with considerable attention being devoted to elucidating the structure, composition, and morphology of the resulting oxide products. The weight change vs time results have usually been reported graphically. With the exception of the linear rate below 700 C and the process of diffusion of interstitial oxygen into the metal,6'9 no effort has been made to characterize the reaction rates in functional form. It is the purpose of this paper to demonstrate that when the fundamental principles of chemical kinetics are rigorously followed, the results of the principal investigations will be correlated and unified and the oxidation rale may be expressed as an analytic function of pressure, temperature, and time. In addition to accounting for the temperature and pressure dependency of the oxidation rate, the following minor features will be accounted for as a result of the basic analysis: the initial period of nonline-arity in rate at low temperatures, which decreases with increasing temperature;3'5'7 the rate vs temperature cusps obtained at constant pressure"5 the concentration gradient of oxygen interstitially dissolved in the metal.5'7 The analysis will also be consistent with the overall chemistry of reaction and with all visual, microscopic, and X-ray observations. DEVELOPMENT OF RATE EQUATION As a fundamental basis for the treatment of metal-oxygen reaction kinetics, it will be regarded that the rate of reaction is determined by the concentration and not the activity or chemical potential. It is further assumed that all metal-oxygen reactions are first order complex chain reactions" whose rate is dependent on the concentration of an intermediate species which is a complex function of the oxygen concentration, or oxygen pressure, only. The basic rate equation is therefore: is the weight of oxygen consumed by the reaction, A is that portion of the area of the metal over which the reaction is occurring (cm2), t the time (sec), kf the rate constant for forward reaction, C the intermediate species concentration and f '([Oz]) and f (Po,) are complex functions of oxygen concentration and Oxygen pressure respectively. Reverse reactions may usually be neglected in metal-oxygen systems since a large negative free energy generally accompanies these reactions. Eq. [I] takes different forms when the rate of reaction is controlled by diffusion into or through a phase or at a phase boundary. For diffusion into the metal phase, the rate is given by1' Di is the diffusion coefficient of species diffusing into the metal phase (cm2/sec), and Q is the corre-

Jan 1, 1962

By R. B. G. Yeo

Pronounced isothermal martensite formation at room temperature was measured dilatometrically in a steel containing 0.01 pct C, 24.9 pct Ni, 0.26 pctAl, 2.58 pct Ti and 0.25 pct Cb. It is shown that martensite will form isothermally if stabilization of the austenite-martensite transformation is eliminated by removal of carbon. The decarburization of two iron-nickel alloys allows isothermal transformation to martensite to occur at temperatures above their athermal Ms temperatures. In an Fe-22.4 pct Ni alloy, at the 0.008 pct C level, the Ms temperature during air cooling is 85°F higher than that during- water quenching-. At the 0.15 pct C level this difference is reduced to only 5°F. The introduction of carbon causes stabilization during air cooling which lowers the Ms temperature virtually to the same level as determined during mate?. quenching. Thus in the 0.15 pct C alloy, the Ms temperature is almost independent of cooling rate. It is suggested that rival theories of martensite formation should be reexamined in alloys of sufficiently low carbon and nitrogen content to eliminate the complication of stabilization. The Ms temperature of a steel containing 0.01 pct C, 24.9 pct Ni, 0.26 pct Al, 1.58 pct Ti and 0.15 pct Cb, solution treated at 1500°F and air cooled as 1/8-in. diam specimens, was found to be 57 °F. 1 However, when held for several hours at room temperature the steel hardened slightly and became appreciably ferromagnetic. Isothermal transformation to martensite was first revealed by Kurdjumov and Maksimova2 in an iron-base alloy containing 0.6 pct C, 6.0 pct Mn and 2 pct Cu. Most of the other studies of isothermal martensite have also been confined to highly alloyed steels which transform at subzero temperatures; for instance, DasGupta and Lement, 3 Cech and Hollomon, 4 Machlin and Cohen,5 Shih, Averbach, and Cohen.6 Averbach and cohen7 noted a rapidly decaying volume increase at room temperature in a steel containing 1 pct C, 1.5 pct Cr and 0.2 pct V. cina8 and Marshall, Perry, and Harpster9 have described the isothermal transformation to martensite at room and subzero temperature in stainless steels. Kurdjumov10 has recently reviewed the subject, noting that the isothermal formation of martensite can be observed only in the temperature range somewhat below Ms or below -50°C. The isothermal formation of martensite may be characterized as follows: 1) It occurs in steels of widely different compositions, the main prerequisite being a low transformation temperature. 2) The transformation occurs by the formation of new plates and not by the growth of old ones. 3) The isothermal transformation is suppresed by stabilization during slow cooling or holding at temperatures near room temperature. However, the factors governing this mode of transformation are still not fully understood. The formation of martensite isothermally suggests an activated process. The early theories of martensite formation did, in fact, utilize classical nucleation concepts. Kurdjumov 11 first proposed the presence of thermally activated nuclei of different sizes and compositions which would grow if they reached critical size during cooling. This treatment was enlarged and developed quantitatively by Fisher, Holloman, and Turnbull12,13 and was later reviewed by the latter two authors.14 Fisher15 associates Ms with a nucleation rate of one per cc per sec. At slightly higher temperatures the nucleation rate is so low that isothermal formation of martensite is not observed in reasonable times. At slightly lower temperatures the nucleation rate is so high that it could not be suppressed by rapid cooling. By judicious use of parameters Fisher 16 was able to obtain good agreement between classical nucleation theory and the incubation times of martensite formation.4 However the application of these principles to martensite formation in iron-nickel alloys15 predicts that an alloy containing about 30 pct (31 at. pet) Ni would not transform. The presence of an Ms temperature at -223° C in an alloy containing 34.1 pct (33 at. pct) Ni led Kaufman and cohen17 to reject the hypothesis of homogeneous nucleation in favor of the reaction path theory originally proposed by Cohen, Machlin and Paranjpe.18 This theory conveniently explains the formation of martensite athermally but becomes labored when dealing with isothermal formation. Kaufman and cohen19 did explain the isothermal activation of embryos by assuming it to be a result of the expansion of their boundary dislocation loops but this treatment predicts an upper temperature limit of isothermal martensite formation.

Jan 1, 1962

By D. J. Stoops

The object of the research described in this paper was to investigate the effect of metallurgical and surface treatments on the corrosion behavior of arc-melted reactor-grade zirconium in cupric or ferric chloride solutions. An apparatus was constructed and specimens of various metallurgical conditions and surface treatments were tested for 6 days at 35° C., with aeration. Some correlations were observed between corrosion rate and the metal's condition and treatment, Specifically, the unattacked or least attacked specimens were those that had been etched as a final treatment before testing. The most severely attacked specimens were those that had been vacuum-annealed as a final treatment before testing. The moderately attacked specimens were those neither vacuum-annealed nor etched, but having a final surface treatment which left a cold-worked surface. Attack by cupric and ferric chloride was by pit- ting with no preference for grain boundaries, The corrosion scale was cow posed predominately of very fine zirconim particles, Particles from the FeC1,-corroded specimens were more pyrophoric than those from CuCl2-corroded specimens, and appeared to have a higher surface area to volume ratio. Comparison of results to those of previous investigators showed that at certain salt concentrations the more pure, reactor-grade zirconium was quite resistant to attack while the less pure, graphite-melted zirconium was severely attacked.

Jan 1, 1962

By T. R. Cass, M. R. Achter

A technique for measuring the creep and rupture strength of nickel specimens bonded by sintered oxide layers has been developed for the investigation of the role of grain-boundary oxide in the oxidation strengthening of nickel during creep at 817 °C. Prom the inverse dependence of the rate of bonding on the thickness of the starting oxide, it is suggested that the rate of diffusion of Ni++ through NiO is the controlling process at the start of sintering. Cornparisons of the creep and rupture strength and of the microstructure of sintered couples with conventionul creep specimens suggest rupture in nickel is prevented by load-bearikzg, ikltergranular layers of oxide. A number of recent investigations have shown that at high temperature and low stress the creep-rupture strength of nickel and nickel-base alloys may be much greater in air than in an inert gas or vacuum.'-7 For example, at 817°C and 2500 psi, nickep failed in vacuum in 48 hr but not in air after 4000 hr, and a Ni-Cr-A1 alloy5 at 1038°C and 3000 psi failed in vacuum in 4 hr but not in air after 731 hr. Fig. 1 is a typical creep curve in air for materials experiencing this pronounced environmental strengthening. A common feature of these curves is the entry into a third stage of accelerating creep, concurrent with the for-

Jan 1, 1962

By M. Kaufman, A. E. Palty

The phase structure and aging characteristics of two nickel-base alloys, Inconel 718 and 702, were investigated. Wrought and cast Inconel 718 showed ArisCb as the major hardening phase, as well as ture was positively identified. Inconel 702 had Ni3Al as the major hardening phase, as well as Cr7C3-of the phase amounts with temperature was determined. 1 HE value of phase structure and aging rate information in the utilization of alloys has been well established. As part of a continuing program, the results obtained on two nickel-base alloys, hconel 718 and Inconel 702, are presented here. Inconel 718 is a relatively new alloy considered for application in both sheet and cast form. Its novelty lies in the use of high columbium tantalum levels in a Ni-Cr-Fe base. No previous work on this type of alloy has been reported in the literature. Inconel 702 is being used now as an oxidation-resistant sheet alloy. Occasional fabrication problems spurred work on its basic structural behavior. The composition of 702 is essentially nichrome plus aluminum and titanium for strengthening and added oxidation resistance. This puts it in the basic class of other nickel-base alloys which have already been studied. The two alloys will be treated separately. INCONEL 718 Phase Study Methods. The phases present after the various conditions investigated were determined by X-ray diffraction analysis of two different elec-trolytically extracted residues and microscopic examination. The extraction methods, using 10 pct HC1 in alcohol and 10 pct H3PO, in water and the X-ray technique have been described previously.' The effect of temperature on the phase behavior was studied on sheet material using the following heat treatments: 2250°F, 2 hr, ice brine quench 1300 100 hr, water quench 2250°F, 2 hr, ice brine quench 1400°, 100 hr, water quench 2250°F, 2 hr, ice brine quench 1500°F, 100 hr, water quench 2250o 2 hr, ice brine quench 1700°F, 48 hr, water quench 2250°F, 2 hr, ice brine quench 1850°, 24 hr, water quench 2250°, 2 hr, ice brine quench 2000°F, 6 hr, water quench The high solution temperature was an attempt to dissolve as many phases as possible without causing melting. Aging exposures were made longer than normal heat treating times in order to approach equilibrium conditions more closely. Cast material was examined only in the as-cast condition and with the normal heat treatment (1700°F, 1 hr, air cool 1325oF, 16 hr,air cool). Materials. The full phase study was performed on sheet specimens approximately 1/2 in. by 2 in. by 1/16 in. The cast pieces were cut from the gating system of a vacuum-cast test piece. An all weld-metal specimen was made by running many weld beads on the sheet using filler made from the sheared edges of the sheet. All external contamination was removed by belt-sanding followed by an electro-polishing treatment. The typical composition of wrought Inco 718 is as follows: The alloy is air-melted. Cast hco 718 may have higher molybdenum. Due to the expectation of finding a Ni-Cb phase (Ni, Cb) for which no X-ray diffraction pattern was available in the ASTM Index, a special 5 Ib heat to the stoichiometric composition of this intermetallic

Jan 1, 1962

By A. H. Daane, B. J. Beaudry

The Sc-Ti system was studied by thermal, metal-lographic, and X-ray methods. Scandium was found to transform at 1334 °C from a (hexagonal) to ß which was concluded to be bee since a continuous series of solid solutions is formed between ß scandium and ß titanium at elevated temperatures. There is a minimum in the solidus at 51 wt pet Ti and 1300°C, a monotectoid at 1050°C and 49 wt pet Ti, and a eutectoid at 875°C and 91.5 wt pet Ti. The maximum solubility of titanium in a scandium is 13.5 wt pet at the monotectoid temperature, while the maximum solubility of scandium in a titanium is 6.5 wt pet at 875°C. SCANDIUM, a member of Group 111 A of the periodic table, and now called a rare-earth metal,' has become of interest recently due to its low density (2.99 g per cc) and relatively high melting point (1539°C).Spedding,' et al. have described a method of preparation of pure scandium metal and have made a study of its basic properties. Since scandium is approximately 10 to 12 pet smaller in at. diam than the other rare earths while its electronegativity and valence are the same, a knowledge of its alloying behavior in contrast to these elements should be very helpful to fundamental alloy theory. Since scandium is quite scarce and difficult to prepare in pure form, its use as a structural material by itself seems quite unlikely. However, its use in special cases as an alloying addi- tive to other low-density materials is a possible application; the Sc-Ti system was chosen for this reason and for others of fundamental interest. Scandium was suspected of having a high temperature bee form as do some of the other rare-earth metals.3'4 Since titanium has a high-temperature bee form, a continuous series of solid solutions at elevated temperatures between ß scandium and ß titanium would prove the existence and structure of the high-temperature form of scandium. The existence of a continuous series of hexagonal solid solutions at room temperature was predicted by Burkhanov and Savitskiy,5 but Hias shown to be incorrect in early X-ray studies. EXPERIMENTAL METHODS Materials. The metals employed in this investigation were crystal bar titanium and distilled scandium prepared by the method described by Spedding,2 et al. The major impurities are listed in Table I in PPm. Alloy Preparation. All the alloys examined were initially formed in a nonconsumable electrode are-melting furnace under an atmosphere of purified helium or argon. A curve based on the observed weight loss of 0.6 pet* when titanium was melted

Jan 1, 1962

By John Fitzpatrick

In this Bureau of Mines investigation a device was developed that permits the determination of the modulus of elasticity of the stress-relief cores obtained in the process of making in situ stress measurements. This determination is made by hydraulically loading the external surface of the stress-relief cores and by measuring the corresponding borehole deformation. The theoretical relationship between the borehole deformation, the applied pressure, and the modulus of elasticity is presented. Also, experimental results obtained from measurements on a simulated stress-relief core made of aluminum and on a limestone stress-relief core are given. Because of the symmetrical loading obtained with this device, the isotropy of the core material can be evaluated. With this device it is also possible to study the effect of eccentricity, that is, the effect within cores in which the inner hole is not coincident with the long axis of the specimen.

Jan 1, 1962

By H. R. Babitzke

The purpose of this investigation was to evaluate the potential of columbium-hafnium alloys as structural materials for use at elevated temperatures. The work described in this report was conducted to determine the properties of columbium-hafnium alloys and to select the more promising ones for further improvement. Properties determined in this report were machinability, hardness, workability, tensile strength, and oxidation resistance. Ten ingots, ranging from 100 percent columbium to 70 atomic-percent hafnium, were prepared and subjected to tests. The test results showed that the alloys with 33 and 50 atomic-percent hafnium were superior in workability, strength, and oxidation resistance. For the alloy series tested, the strength and hardness values increased with the increasing hafnium content. Maximum values were reached with 50 atomic-percent hafnium. The oxidation resistance was poorest at the 1 atomic-percent hafnium level but improved with increasing hafnium content through 70 atomic-percent. Eight of the ten ingots were fabricable at room temperature. The two remaining ingots, those with 5 and 10 atomic-percent hafnium, required hot-working.

Jan 1, 1962

By Harold Margalin, Elmars Ence

M. H. Mueller, M. V. Nevitt, and H. W. Knott (Argonne National Laboratory)—We have reported1 the crystal structure of Ti2CU as body centered tetragonal with a. = 2.944A and co = 10.786A, six atoms per unit cell, and space groupl4/mmm(MoSi2 type). This cell is larger but definitely related to the unit cell reported by the authors. It permits definite positions for the titanium and copper atoms in the cell located as follows: 2 Cu (a) 0 0 0; 1/2 1/2 1/2 4 Ti (e) 0 0 z; 1/2 1/2 1/2 + z; 0 0z; 1/2 1/2 1/2- z where z = 0.341 The face centered tetragonal cell reported by the authors can be transformed to a small body centered tetragonal cell with flo (small bet) = ao(fct)v2 Both unit cells have the same CO. Neither the face centered tetragonal cell with four atoms per unit cell nor the small body centered tetragonal cell with its two atoms per unit cell lend themselves conveniently to an orderly arrangment of the 2 to 1 ratio of titanium to copper atoms. When the co of this small body centered cell is tripled, however, a large body centered tetragonal cell results with six atoms per unit cell as described above. We had also noted that the X-ray patterns of Ti2Cu indicated that the structure could be approximately described by the face centered tetragonal cell as reported by the authors; how- ever, there was evidence for a few additional very weak lines whose positions indicated a larger unit cell. Since the X-ray scattering amplitudes of titanium and copper are nearly equal, it is evident that it is difficult to distinguish their positions especially from X-ray powder patterns. It was therefore decided to look at a powder pattern obtained by neutron diffraction since the scattering amplitudes of the two elements are considerably different in magnitude and opposite in sign. The sample used for neutron diffraction was selected from a group of three alloys prepared by arc melting using crystal bar titanium of 99.92 pet nominal purity and 99.999 pet pure Cu. The alloys designated as A, B, and C had the following respective compositions: Ti-32.8 at. pet Cu, Ti-33.3 at. pet Cu, and Ti-33.8 at. pet Cu. On the basis of the melting losses incurred, it was established that the actual concentration of either component in any of the alloys probably did not deviate from the intended value by as much as 0.1 at. pet. The alloys were annealed for 5 days at 700°C in evacuated Vycor capsules and quenched in tap water. The metallographic structures of these alloys are shown in Fig. 1. None of the alloys contained sufficient second phase to permit its positive identification. Since alloy B contained the least amount of second phase and since its composition placed it closest to the ideal stoichiometry, it was chosen for the neutron diffraction study. The oxygen content of alloy B was found by chemical analysis to be 0.06 at. pet. This particular intermetallic compound is especially suitable for investigation with neutron diffraction since if the titanium and copper atoms have a random statistical distribution, a near null-matrix would result in which there would be practically no coherent scattering of neutrons, and hence no Bragg diffraction peaks. Such a condition could come

Jan 1, 1962

By Morris Cohen

STAFF: Editor, Gerhard Derge Acting Editor, Paul G. Shewmon Carnegie Institute of Technology Schenley Park Pittsburgh 13, Pa. Editorial Assistant, M. A. Redmerski Production Editor, Otto T. Johnson THE METALLURGICAL SOCIETY: Karl L. Fetters, President; J.S. Smart, Jr., Past-President; R. C. Cole, Vice President; R. L. Hennebach, Treasurer; R. W. Shearman, Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: W. O. Phil-brook, Chairman; H. L. Bishop, R. C. Cole, J. N. Hobstetter, W. A. Krivsky, E. R. Morgan, F. C. Langenberg, R. E. Lund, Paul Queneau, L. L. Seigle, R. L. Smith, and T. V. Wainwright. Review and selection of manuscripts is under the supervision of the following Publicotions Committes: Extractive Metallurgy Division: R. E. Lund, Chairman; M. E. Wadsworth, Vice Chairman; D. H. Baker, Jr., G. M. Bell, R. E. Grace, W. A. Krivsky, R. A. Lewis, Charles O'Neill, A. W. Schlechten, R. E. Shinkoskey, and W. W. Stephens. Iran and Steel Division: T. V. Wainright, Choirman; H. L. Bishop, R. E. Boni, T. E. Dancy, D. W. Murphy, Johannes M. Uys, J. B. Wogstoff, and R. G. Ward. Institute of Metals Division: J. N. Hobstetter, Chairman; P. A. Beck, J. J. Becker, G. F. Bolling, J. 0. Brittain, J. B. Clark, R. S. Davis, A. E. Dwight, R. W. Fountain, L. R. Girifolco, J. C. Gurland, H. S. Kalish, E. L. Harmon, J. J. Heger, A. A. Hendrickson, L. Himmel, J. P. Hirth, H. H. Johnson, Jr., R. R. Nosh, T. N. Rhodin, R. H. Richman, H. C. Rogers, W. Rostoker, C. Sherby, C. W. Spencer, L. Slifkin, J. K. Stanley, R. Steinitz, H. C. Stumpf, and R. Swalin. Published bimonthly by the Americon Institute of Mining, Metallurgicol, and Petroleum Engineers, Inc., 345 East 47th Street, New York 17, N. Y. Telephone PLaza 2-6800. Subscription $30 peryear for non-AIME members in United States and North, South, and Centrol America; $32, foreign; $30per$7.50 for AlME members. Single copies, $6.00, single copies foreign, $6.50. The AlME is not responsible for any stotement made or opinion expressed in its publications ... Copyright 1962 by the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . . . Registered cable address, AlME New York . . . Indexed in Engineering Index, Industrial Arts Index, and Chemical Abstracts . . . Second class postage paid at New York, N. Y., and Ann Arbor, Mich. Volume 224, Number 4.

Jan 1, 1962

By H. O. Seigel

Induced Polarization includes many types of dipolar charge distributions set up by the passage of current through consolidated or unconsolidated rocks. Among its causes are concentration polarization and electrokinetic effects in all rocks and the phenomenon of Overvoltage in rocks containing electronic conductors such as metallic sulphides and graphite. In normal rocks the polarization effects may be usually con-fined within relatively narrow limits and any large departures may be at-tributable to the presence of electronic conductors. In practice, Induced Polarization is measured in one of two ways. In the first a steady current of some seconds duration is passed and abruptly interrupted and the slowly decaying transient voltages existing in the ~round are measured after interruption. This is known as the "pulse", "transient", or Direct Cur-rent Induced Polarization (D.C.I.P.).The second method entails a comparison of apparent resistivities using sinusoidal alternating current of two or more frequencies, generally within the range of 1/10 to 10 c.p.s. Induced Polarization extends the

Jan 1, 1962

By L. G. Marshall

This report is one of a series published by the Federal Bureau of Mines, describing mining methods and performance at individual mining operations throughout the United States. The objective of these papers is to promote development and conservation of our mineral resources by disseminating reliable technological information on mining methods, practices, and performance. Limestone deposits in Iowa are extensive and reserves are large. Most of the past production came from the eastern third of the state, although over half of the counties in the state have produced, or are now producing limestone. The stone is used as aggregate, road metal, agricultural lime, riprap, fluxing stone, railroad ballast, and in the manufacture of cement and lime.

Jan 1, 1962

By R. Maddin, A. Lawley

Single crystal Mo-Re alloys (99.99+ purity), grown by electron bombardment floating zone heating, were deformed in tension at temperatures from -196° to +200°C. At -196oC, Mo-6 pet Re and Mo-20 pct Re alloys deform by slip on systems of the type (101) [1ll]. Above-78oC, the operative slip system is of the type (112) [111], (101) [1ll], or (211) [1ll], depending upon orientation. Mo-39 pct Re alloys deform by twinning and slip at all test temperatures with a (112) [111] type twinning system. Critical resolved shear stress for slip and twinning is calculated as a function of composition and temperature, and the mechanical properties compared with those of less Pure polycrystalline alloys. HEXAGONAL close-packed rhenium, c/a = 1.615, is highly soluble in molybdenum. The bee molybdenum-rich solid solution extends to approximately 42 at. pet Re* at 2500°C,' Fig. 1. Recent work on polycrystalline alloys has shown conclusively that the addition of rhenium to molybdenum improves both the fabricability and the low-temperature ductility.2"5 Similar behavior is observed for W-Re and Cr-Re alloys.5 Initially, Geach and Hughes2 found that the Mo-30 pct Re alloy could be cold rolled to approximately 90 pct reduction before the onset of cracking. The remarkable effect of the rhenium was later confirmed by Jaffee et al. 3-5 with an optimum condition of maximum strength combined with maximum ductility at the Mo-35 pet composition. At higher rhenium contents, the ductility was severely impaired due apparently to the presence of brittle tetragonal s phase, Fig. 1. In the Mo-35 pet Re alloy, at least 110 ppm (parts per million) oxygen could be tolerated before cold workability was reduced. By comparison, the corresponding tolerance figure in unalloyed molybdenum is ~ 10 ppm. The effect of rhenium was considered in terms of: 1) a reduction in oxygen solubility in the lattice; 2) a redistribution of intergranular oxide from grain boundary films to isolated spheres; and 3) the promotion of twinning as a further mode of plastic deformation. Paradoxically, twinning is often associated with brittle fracture in iron and the silicon irons.6'7 Work to date has been restricted to are-melted and powder metallurgy polycrystalline material of ~ 99.9 pet purity. The present investigation was initiated for the purpose of determining the mode and crystallography of plastic deformation of a series of bee Mo-Re alloy single crystals over a wide temperature range from -196o to +200°C. Using high-purity zone-melted material (~ 99.99 + pet purity), the specific role of rhenium in the molybdenum lattice may be understood more fully since effects due to grain boundaries and oxide redistribution will be absent. At the same time, the study provides a comparison of single and polycrystalline deformation behavior. EXPERIMENTAL TECHNIQUES A) Preparation and Purity of Single Crystals. Alloys in the form of either are-cast and swaged or sintered and ground bar, 0.120 in. diam, were obtained from the Chase Brass and Copper Co. Alloy single crystals ~ 8-in. long were grown from the

Jan 1, 1962

By E. W. Lucht

THE term "high pressure", as used in industry today, is applied rather loosely. Generally, it refers to pressures that are higher than those encountered in most industrial processes although no definite limits are normally stated. For the purpose of this talk I should like to set rather arbitrary limits to the term "high pressure", and in ab-solute figures this would be the range from 1000 psi to perhaps 40,000 or 50,000 p.s.i. The scope of high pressure technology is very broad, and it would take more time than we have avail-able here today to cover fully even one aspect of the field. Therefore, I should like to discuss just some of the techniques used and problems en-countered in high pressure operations. Research work into the high pressure region dates back about 150 years, but it was not until 1910 that the first commercial application of high pressure technology was made in the production of ammonia.

Jan 1, 1962