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By C. G. Dunn, J. L. Walter

SILICON-iron .under certain conditions of processing and annealing will form a cube texture. The occurrence of this texture in thin tapes of silicon iron was first reported by Assmus, Detert, and Ibe.' They concluded that the cube texture in their material formed by a secondary re crystallization process. In the course of present investigations on the development of the cube texture and the mechanisms involved in its formation by secondary re-crystallization it was found that under certain conditions the cube texture was replaced by a cube-on-edge or (110) [001] texture. We call this phenomenon tertiary re crystallization since it follows secondary recrystallization. The secondary recrystallization occurs after primary recrystallization and a substantial amount of normal grain growth. It is the purpose of this paper to describe briefly the occurrence of tertiary recrystallization and the structure and texture prior to and after tertiary recrystallization. The primary and secondary recrystallization structures and textures are the subject of another study and will be referred to briefly in the discussion of results. Evidence will be presented for the view that the dominant driving force for tertiary recrystallization is derived from the surface free energy which depends on the crystallographic planes presented to the gas-metal interface. In the absence of boundary restraining forces (dispersed phases, thermal grooves, and so forth) a sufficiently large difference in surface free energy across a grain boundary would produce boundary migration away from the center of curvature of the boundary intersection line in the surface of the sample according to risher.2 Therefore, particular attention was paid to observation of the direction of motion of these surface boundary lines. Furthermore, measurements of the actual boundary curvatures could be used to estimate the driving force supplied by surface free energy. EXPERIMENTAL PROCEDURE Samples were prepared by hot and cold-rolling vacuum-melted ingots of iron containing 3 pct Si to strips 0.012 and 0.006 in. thick. The ingots contained less than 0.005 wt pct impurities. The rolled strips were cut into samples approximately 1 in. wide by 3 in. long and were electropolished to remove surface imperfections. All samples were annealed in a vacuum at a pressure of approxi-

Jan 1, 1960

By R. D. Pehlke, J. F. Elliott

The equilibrium pressure of nitrogen gas over pure silicon metal and silicon nitride has been measured in the temperature range 1400° to 1700°C. From the experimental data, the standard free energies and enthalpies of formation of Si3N4(a) have been calculated as functions of temperature over the above temperature range. Utilizing data in the literature and the results of this investigation, the specific heat, molar enthalpy, molar entropy, standard enthalpy of fornation, and standard free energy of fornation are estimated for the temperature range 298° to 1400°C. THE high-temperature thermodynamic properties of many metallic nitrides are not well established at present. This is a serious deficiency because nitrogen and nitride-forming metals are important alloying additions to steels, and knowledge of the interaction between nitrogen and these elements is essential to a better understanding of the behavior of steels. Metallic nitrides also are used as refractory materials. Consequently, the investigation reported here was undertaken to provide more complete information on the standard entropy and free energy of formation of silicon nitride. The experimental technique provided a direct measurement of the equilibrium pressure of nitrogen gas in the range of 1413 to 1700°C for the reaction: 3 Si(1) + 2N2 (g) = Si3N4 (a) [ 1 ] and below 1413oC for the reaction: 3Si(c) + 2N2(g) = Si3N4(a) [2] APPARATUS The experimental system consisted of a crucible assembly, a reaction chamber, and a gas supply and vacuum system. The Crucible Assembly which contained the equilibration specimen and molybdenum radiation shields with a susceptor for induction heating is shown in Fig. 1. Two covered, high-purity alumina crucibles, one nested within the other, contained the susceptor, shields and specimen. Central openings in the upper shield and crucible covers permitted on optical pyrometer to be sighted into the central cavity of the specimen. The specimen itself was a 5/8 OD by 1-in.

Jan 1, 1960

By M. Cohen, C. Wagner, J. E. Reynolds

If the total volume of a diffusion couple changes during the diffusion, the measurement of distance becomes ambiguous. Use of distance parameters as suggested by Hartley and Crank is discussed. For small concentration differences, the standard form of Fick's second law is retained with conventional length units and the in- terdiffusion coefficient D. It is shown how D can be calculated from experiments involving large concentration differences and analyzed in terms of distance parameters. 'The merits of incremental diffusion couples involving small concentration differences are emphasized. THE conventional form of Fick's second law for one-dimensional diffusion of component B in a binary solution of A and B is where c, is the concentration of component B; x, the distance; t, the time; and D, the interdiffusion coefficient which may depend on ca. Hartley and Crank' have pointed out that Eq. 1 applies only if the total volume of the diffusion couple does not change during the diffusion process; otherwise, the definition of x becomes ambiguous. No change in total volume takes place if the specific volume of the solution is a linear function of the weight fraction Wb, or if the molar volume is a linear function of the mol fraction N. In some alloys, however, these relationships do not hold, and then it is necessary to introduce a modified measure of distance, 4 in order to retain the general form of Eq. 1. The application of Hartley and Crank's suggestions to diffusion in alloys has been discussed by Wagner.' Relation Between Measure of Distance and Units of Concentration The definition of [ depends on the choice of units for the concentration c,, as follows: 1—If the concentration ca is measured as the weight fraction W, (or weight percent), [ = 5, has to be defined so that equal increments of contain equal increments of mass m of the solution, e.g., dm = pSdx = Sdw [2] where p is the local density of the solution, and S is the cross-sectional area in sq cm which is taken to be constant in this problem of one-dimensional diffusion." * da Silva and Mehla have demonstrated the constancy of the cross-sectional area in the usual type of diffusion couple. However, experiments involving diffusion into thin wires4, 5 may exhibit changes in cross-sectional area, and therefore are excluded from the present treatment. Thus and the unit of is gram per sq cm instead of cm. 2—If the concentration c, is the mol fraction N, must be defined so that equal increments of contain equal numbers of mols of solution, e.g., dn= (S/V)dx= Sd [41 where V is the local molar volume of the solution. Thus dt, = dx/V [51 and the unit of is mols per sq cm. 3—If, as may be advisable in the case of interstitial solutions, the concentration C is measured in terms of the molar ratio of components B and A (c,, = Y, = nH/nA, where n and nl are numbers of mols of B and A), = Y has to be defined so that equal increments of contain equal numbers of mols of A, e.g., dnA= (NAS/V)dx = Sdf [6]

Jan 1, 1954

By I. W. Alcorn

The cost of drilling in the past few years of proration and ever decreasing allowables has received increasing thought and study. It seems to parallel the strides made with respect to pumping problems in 1932 and 1933. Low profit margins stimulate the search for economies. Any discussion of slim-hole drilling involves a multitude of abstract values, and the problem can be attacked only by a study of records and rational thinking. In a measure, traditional methods must be studied with a questioning attitude. The words "slim hole" may be somewhat misleading, as the term is entirely relative. For that reason I wish to define it as used in this discussion. On the Gulf Coast, I would define a normal hole as one in which 10 3/4-in. surface casing has been set and below which a 9 7/8-in. hole is dug. With this as a datum, holes of larger diameter below surface would be called "large holes," with 121/4 in. as the "extra large" class and holes of smaller diameter classed in the slim-hole range, 6 1/4 in. representing about the minimum size. The optimum size has not been definitely determined, but the preference is for a program that would call for setting 8 5/8 -in. surface casing and digging a 7 3/4 - in. hole. Different sections of the country might very properly deviate from this practice because of differences in depth, formations, regulations, or other factors. This paper will be confined to a discussion of the drilling of exploratory wells, as the drilling of this class of wells is quite a different problem from that of drilling a proven field, although many of the same considerations apply in both cases, as will be apparent. Although for many years shallow slim-hole and core-test holes of small diameter had been dug, it was not, I believe, until the fall of 1937 that serious consideration was given to its application in drilling wells 7000 ft., 8000 ft. and 9000 ft. deep on the Gulf Coast. This does not mean that nearly all such wells drilled on the Gulf Coast now are of the slim-hole variety, but only that efforts have been aimed in that direction with very encouraging results and there has been a very definite trend to reduce the size of holes, a trend that probably will continue. As to exploration policy, there appear to be two distinct and opposite views. The one usually followed in the past was more or less designed to "shoot the works" on one well. Generally on the Gulf Coast, the depth at which production might be obtained is limited by the drilling equipment and economics. With this thought in mind, wildcat wells are often planned with the idea of carrying the depth to 10,000 It., or even 15,000 ft. All of the possible hazards are anticipated and the general drilling and casing programs are so predicated. Such wells contemplate the drilling of large-diameter holes; the setting of at least one protective string of casing and an extensive coring policy, all of which finally adds up to an expensive well. AS opposed to this general policy is the slim hole. This, on the Gulf Coast, recognizes that new discoveries represent gam-

Jan 1, 1941

By I. W. Alcorn

The cost of drilling in the past few years of proration and ever decreasing allowables has received increasing thought and study. It seems to parallel the strides made with respect to pumping problems in 1932 and 1933. Low profit margins stimulate the search for economies. Any discussion of slim-hole drilling involves a multitude of abstract values, and the problem can be attacked only by a study of records and rational thinking. In a measure, traditional methods must be studied with a questioning attitude. The words "slim hole" may be somewhat misleading, as the term is entirely relative. For that reason I wish to define it as used in this discussion. On the Gulf Coast, I would define a normal hole as one in which 10 3/4-in. surface casing has been set and below which a 9 7/8-in. hole is dug. With this as a datum, holes of larger diameter below surface would be called "large holes," with 121/4 in. as the "extra large" class and holes of smaller diameter classed in the slim-hole range, 6 1/4 in. representing about the minimum size. The optimum size has not been definitely determined, but the preference is for a program that would call for setting 8 5/8 -in. surface casing and digging a 7 3/4 - in. hole. Different sections of the country might very properly deviate from this practice because of differences in depth, formations, regulations, or other factors. This paper will be confined to a discussion of the drilling of exploratory wells, as the drilling of this class of wells is quite a different problem from that of drilling a proven field, although many of the same considerations apply in both cases, as will be apparent. Although for many years shallow slim-hole and core-test holes of small diameter had been dug, it was not, I believe, until the fall of 1937 that serious consideration was given to its application in drilling wells 7000 ft., 8000 ft. and 9000 ft. deep on the Gulf Coast. This does not mean that nearly all such wells drilled on the Gulf Coast now are of the slim-hole variety, but only that efforts have been aimed in that direction with very encouraging results and there has been a very definite trend to reduce the size of holes, a trend that probably will continue. As to exploration policy, there appear to be two distinct and opposite views. The one usually followed in the past was more or less designed to "shoot the works" on one well. Generally on the Gulf Coast, the depth at which production might be obtained is limited by the drilling equipment and economics. With this thought in mind, wildcat wells are often planned with the idea of carrying the depth to 10,000 It., or even 15,000 ft. All of the possible hazards are anticipated and the general drilling and casing programs are so predicated. Such wells contemplate the drilling of large-diameter holes; the setting of at least one protective string of casing and an extensive coring policy, all of which finally adds up to an expensive well. AS opposed to this general policy is the slim hole. This, on the Gulf Coast, recognizes that new discoveries represent gam-

Jan 1, 1941

By R. Simon, L. Yarborough

This paper presents a correlation for predicting the critical pressures of gas-solvent-reservoir oil systems of the type encountered in gas and solvent injection processes. Experimental data from 14 systems were used to develop the correlation which expresses critical pressure as a function of composition, C7+ mol weight, and C7+ characterization factor. Critical pressures predicted by the correlation for the 14 gas-solvent-reservoir oil systems have an average deviation of 2.8 per cent of the experimental values. The correlation war used to study a wide variety of other hydrocarbon mixtures reported in the literature whose critical conditions are in the range of interest in oil recovery work (100 to 280F and 2,000 to 6,000 psia). Critical pressures predicted by the correlation had an average deviation, expressed as per cent of experimental value, of 5 per cent for 20 miscellaneous mixtures from the literature, and 6.4 per cent for I7 methane-butane-decane mixtures reported by Sage and Lucey. INTRODUCTION Predicting critical points of hydrocarbon mixtures is an important part of phase behavior calculations. If the critical point can be predicted for a specific mixture, the separation between the bubble-point and dew-point regions will be defined, and physical properties of the mixture can be calculated by using the principle of corresponding states. Numerous correlations for predicting critical points of hydrocarbon mixtures have been published. Six of these correlationsl-8 were for light hydrocarbons, and two correlations7,8 ere for high boiling-point petroleum distillates. Organick9 And Eilerts" presented correlations which combined the published data from both light and heavy mixtures, and these correlations became the only available methods for predicting critical pressures for wide boiling range mixtures. In the course of the authors' work on secondary recovery by gas and solvent injection, experimental data were obtained for 14 mixtures of dry gas, ethane-propane-butane solvents, and various reservoir oils. The critical pressures and critical temperatures of these gas-solvent-reservoir oil systems were in the range of 1,900 to 4,800 psia and 180 to 265F. The critical pressures predicted for the 14 mixtures by the correlations of Organick and Eilerts had an average deviation from the measured values of about 13 per cent. The authors felt that it was necessary to develop a better correlation for engineering calculations and the resultant correlation, which is presented on Figs. 1 and 2, predicts the critical pressures of the 14 mixtures with an average deviation of 2.8 per cent. The validity of the correlation was tested by applying the correlation to other hydrocarbon mixtures reported in the literature. This subject is discussed later in the paper. The authors feel that there is also a need for an improved critical temperature correlation for gas-solvent-reservoir oil systems. However, developing a critical temperature correlation is a significant study in itself and is not included in this paper. EXPERIMENTAL DATA The compositions and critical points obtained by the authors for 14 gas-solvent-reservoir oil mixtures are shown on Table 1. The methane concentrations in these mixtures varied from 20 to 63 mol per cent. The intermediate hydrocarbon group, consisting of ethane, propane, and butane, varied from 20 to 64 mol per cent, and the concentration of the C,, fraction from 10 to 20 mol per cent. The physical properties of the C,, fraction covered the range from light, paraffinic, nonasphaltic (Mixtures 5, 6, 7, 8, 9 and 10) to heavy, aromatic, and asphaltic (Mixtures 13 and 14).

By I. W. Alcorn

THE cost of drilling in the past few years of proration and ever decreasing allowables has received increasing thought and study. It seems to parallel the strides made with respect to pumping problems in 1932 and 1933. Low profit margins stimulate the search for economies. Any discussion of slim-hole drilling involves a multitude of abstract values, and the problem can be attacked only by a study of records and rational thinking. In a measure, traditional methods must be studied with a questioning attitude. The words "slim hole" may be somewhat misleading, as the term is entirely relative. For that reason I wish to define it as used in this discussion. On the Gulf Coast, I would define a normal hole as one in which 10 3/4-in. surface casing has been set and below which a 9 7/8-in. hole is dug. With this as a datum, holes of larger diameter below surface would be called "large holes," with 12 1/4 in. as the "extra large" class and holes of smaller diameter classed in the slim-hole range, 6 1/4 in. representing about the minimum size. The optimum size has not been definitely determined, but the preference is for a program that would call for setting 8 5/8-in. surface casing and digging a 7 3/4-in. hole. Different sections of the country might very properly deviate from this practice because of differences in depth, formations, regulations, or other factors. This paper will be confined to a discussion of the drilling of exploratory wells, as the drilling of this class of wells is quite a different problem from that of drilling a proven field, although many of the same considerations apply in both cases, as will be apparent. Although for many years shallow slim-hole and core-test holes of small diameter had been dug, it was not, I believe, until the fall of 1937 that serious consideration was given to its application in drilling wells 7000 ft., 8000 ft. and 9000 ft. deep on the Gulf Coast. This does not mean that nearly all such wells drilled on the Gulf Coast now are of the slim-hole variety, but only that efforts have been aimed in that direction with very encouraging results and there has been a very definite trend to reduce the size of holes, a trend that probably will continue. As to exploration policy, there appear to be two distinct and opposite views. The one usually followed in the past was more or less designed to "shoot the works" on one well. Generally on the Gulf Coast, the depth at which production might be obtained is limited by the drilling equipment and economics. With this thought in mind, wildcat wells are often planned with the idea of carrying the depth to 10,000 ft., or even 15,000 ft. All of the possible hazards are anticipated and the general drilling and casing programs are so predicated. Such wells contemplate the drilling of large-diameter holes; the setting of at least one protective string of casing and an extensive coring policy, all of which finally adds up to an expensive well. As opposed to this general policy is the slim hole. This, on the Gulf Coast, recognizes that new discoveries represent gam-

Jan 1, 1941

By H. H. Hausner, H. S. Kalish

M. Hansen—This paper certainly is an interesting study. Although I have not had too much experience in the powder metallurgical methods of studying phase equilibria, I would like to say the following concerning the interpretations of the results obtained: 1. The existence of a zirconium-rich eutectic having a melting point close to 950°C and containing approximately 5 pct beryllium is well established. 2. Undoubtedly sintering of the original compacts (i.e., without repressing and resintering at 1350°C) resulted in a condition being far from equilibrium, even in the low-melting point zircon-rich region where undissolved zirconium particles have been observed. This means that only partial reaction between the component powders has taken place. 3. In preparing and handling powder mixtures for pressing and sintering, we have found that with powders differing considerably in density, and also in particle size, separation in layers of different composition may occur. This means that a concentration gradient would exist within such samples. This phenomenon may, at least to some extent, account for the difference in microstructure of the top and bottom regions of some of the sintered samples. If this is the case, density figures for some of the nominal compositions would not represent actual densities of those mixtures. 4. Fig. 1 shows that the low densities of mixtures with 40 and 60 pct beryllium sintered at 1350°C are changed to much higher densities if the products sintered at 1100°C are repressed and resintered at 1350°C, whereby an approach toward equilibrium takes place. This would mean that the low density and growth in volume is due to nonequilibrium conditions. If this is true, would it be justified, then, to conclude that "the remarkable growth of the alloys in the vicinity of 40 to 60 pct Be indicates the formation of a high-melting point phase, probably accompanied by a considerable change in volume due to a large alteration of the crystal structure from that of the original compounds"? If some compound formation has taken place already during the first sintering at 950" to 1350°C, more compound would be formed by repressing and re-sintering of the 1100" samples. This treatment, however, results in higher, rather than lower, densities. In general, the density-composition curve of alloy systems containing one or more intermediate phases is characterized by a more or less defined contraction (decrease in specific volume, increase in density) over the "theoretical" density. Does not discrepancy exist between the two statements that "growth of the alloy indicates the formation of a high-melting phase . . ." and "even at 1350°C, no indications of sintering have been observed"? 5. I am not sure that the explanation given for the fact that fig. 4 did not reveal as much eutectic as the top portions of the mixture with 2 pct Be, is correct. The density of the melt containing only 5 pct Be or even perhaps less, is not too much different from that of the nominal composition. The reason might be also that there was already some separation of the components in the pressed compact. 6. I do not understand why the microstructure of the bottom regions of the compact with 5 pct Be (fig. 6) is so different from that of the top regions (fig. 5). The compact was melted on sintering at 1100°C. Its composition lies close to the eutectic point. There should be at least some lamellar structure in the bottom regions too; otherwise, the composition of top and bottom must have been very different after sintering, because the eutectic is said to extend as far as the composition ZrBe2. In case the white and gray areas of fig. 6 are both gamma, and the black areas undissolved zirconium, this composition would be close to the phase coexisting with zirconium, that is, ZrBe2, according to the hypothetical diagram, or a compound richer in zirconium. 7. Figs. 9 and 10 are not mentioned in the text. 8. The great difference in microstructure of the composition 20 pct Be of figs. 8 and 14 on one side and fig. 15 on the other side proves that sintering at 950" and 1100°C results only in partial reaction of the powers. 9. The mixture with 60 pct Be (fig. 19) seems to consist of two phases, rather than one phase, one interspersed in a matrix of another. 10. The statement that the eta phase "may be an intermetallic compound or the product of a peritectic or monotectic reaction" seems to be misleading, because the product of a peritectic or monotectic reaction in this region of the system must be an intermetallic compound. 11. If there is some solid solubility of Be in alpha and beta-Zr, it would be expected to be higher in beta-Zr (b.c.c.) than in alpha-Zr (h.c.p.). The temperature of the polymorphic transformation of zirconium then would be lowered, rather than increased. In accordance with this, Battelle has found that the transformation point of titanium is decreased by beryllium. 12. In case the phases present in alloys with 80, 90, and 95 pct Be are identical (which appears to be correct), it is striking that the relative amounts of both phases (eta and beryllium) are not too different within this wide range of composition. With 60 to 65 pct Be

Jan 1, 1951

By C. L. T. Edwards

IN the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on 100 per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer's further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blast-furnace charge as good iron as that made without scrap-made with straight ore?" This question may be answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on 100 per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. OPERATION WITH 100 PER CENT STEEL SCRAP During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a 100 per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when l00 per cent steel turnings were charged. Except for occasional charges of nickel scale as an "extra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore-ore and scrap-operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from i00 per cent scrap to the regular burden, the charge hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap charge. The furnace employed had a hearth 16 ft. 0 in., bosh 22 ft. 0 in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter ¾ in., bosh angle 73° 27' and a Baker-Neuman top, with gas-engine blowers. Analyses Range of Material Charged Gravel: Si02, 64.40 to .7o.54 per cent; A1203,3-52 to 4.58; CaO, 7.27 to 9.49; M90, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83.

Jan 1, 1941

By P. Beardmore, B. W. Howlett, B. D. Lichter, M. B. Bever

The heats of formation at 273°K of the compounds Mg2Ge, Mg2sn, and Mg2b, the heats of fusion and melting points of Mg2Sn and Mg2Pb, and the heats of solution of magnesium, germanium, and lead in liquid tin have been measured. The excess free energies of the liquid alloys and the free energies of formation of magnesium-Group IVB compounds at their melting points and their standard free energies of formation at 298°K have been calculated. The stability and bonding of the compounds are discussed with reference to these properties. Some thermodynatnic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. THE compounds of magnesium with the Group TVB elements, silicon, germanium, tin, and lead, have often been considered to constitute a nearly ideal homologous series. In particular, their thermodynamic stability has been assumed to decrease with increasing atomic number of the Group IVB element.' The binary-phase diagrams of the magnesium-Group IVB elements given by Hansen and Anderko2 have the same form. Each system has a single con-gruently melting compound of limited homogeneity range. The structures of these compounds, which have the formula Mg2X, are anti-isomorphous with the calcium fluoride structure. A recent investigation has found evidence of a second compound in the system Mg-Pb.3 The solid compounds Mg2Si, Mg2Ge, and Mg,Sn are semiconductors, while the conductivity of Mg2Pb approaches that of a metallic conductor. This difference suggests that other properties may also show a discontinuity. The investigation reported here is concerned with the thermodynamic properties of magnesium-IVB compounds and particularly their variations with the period of the Group IVB element. The heats of formation at 273°K of the compounds MgzGe, Mg2Sn, and Mg2Pb and the heats of fusion and melting points of Mg2Sn and Mg2Pb have been measured. The results, combined with published data, are interpreted in relation to the stability and the bonding characteristics of the compounds. Some thermodynamic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. In the course of the investigation the heats of solution of magnesium, germanium, and lead in liquid tin have been determined. 1) EXPERIMENTAL PROCEDURES 1.1) Samples. Samples of the compounds Mg2Ge, Mg2Sn, and Mg2Pb, supplied by Professor P. Aigrain, Compagnie Générale de Télégraphie Sans Fils, were used in measuring heats of formation, heats of fusion, and melting points. Samples of Mg2Sn and Mg2Pb, supplied by Dr. V. B. Kurfman, Dow Metal Products Co., samples of Mg2Sn, prepared at the Air Force Cambridge Research Laboratories, and samples of MgzPb, prepared in this laboratory, were used for additional measurements of the heats of fusion and the melting points. The samples were stored in evacuated Pyrex capsules or under nonreacting liquids. 1.2) Heats of Formation. The heats of formation at 273°Kof the compounds Mg2Ge, Mg2Sn, and Mg,Pb were measured by tin-solution calorimetry. In this method, samples of the compound and of a mixture of the constituent elements are added alternately from 0°C to a tin-rich bath. The difference between the heat effects, corrected for the change in composition of the bath, is the heat of formation of the compound. Details of the method have been given elsewhere. 4 The bath was maintained at 350°C for the dissolution of the compounds MgzSn and Mg2Pb. Since at this temperature the dissolution of Mg2Ge was too slow, a bath temperature of 400" or 450°C was used with this compound. At least three calorimetric runs, each of approximately six additions, were made with each compound. 1.3) Heats of Solution. The determination of the heats of solution of magnesium, germanium, and lead in tin was included in this investigation because they were not well-established at the time this work was started. To obtain the heat of solution, the difference

Jan 1, 1967

By AIME AIME

A JOINT meeting of the Canadian Institute of Mining and Metallurgy and the American Institute of Mining and Metallurgical Engineers was held at Spokane, Wash., and Cranbrook and Kimberley, B. C., on Oct. 13 to 16, 1926, with a total attendance at one or another or all of the meetings of about 300 members, ladies and guests. At the opening meeting, on Oct. 13, in the Davenport Hotel, Spokane, about 175 were present. The morning was occupied with addresses of welcome by M. H. Sullivan for the Columbia Section, who called on Mayor Charles A. Fleming, President John F. Davies for the Chamber of Commerce, and E. R. Hannibal, president of the Associated Engineers, each of whom heartily welcomed the visitors. Philip N. Moore, former president, and special representative of President Samuel A. Taylor, replied for the A.I.M.E., and Lewis Stockett, president, and Charles A. Banks, chairman, British Columbia Division, Canadian Institute of Mining and Metallurgy, and Henry M. Parks for the visiting A.I.M.E. sections, made appropriate responses on behalf of those they represented. The members and ladies had luncheon with the Associated Engineers. Philip N. Moore addressed the assembly on "The Opportunity of the Engineer"; an excerpt from his address appears on another page. At the afternoon meeting, with Lewis Stockett in the chair, Frank M. Smith was asked to make a brief statement of the proceedings of the Silver Producers Association in Denver. Supplementing his talk by placing a well-prepared statement on "Silver and the Plan of the Royal Commission on Indian Currency and Finance" in the hands of those present, he narrated what had been undertaken by the Silver Producers Association and what they hoped to accomplish.

Jan 1, 1926

A. W. TRACY' AND D. H. THOMPSON (presented in written form).-Messrs. Ed¬munds, Anderson and Waring are to be commended for their excellent work in so painstakingly reducing to constants, the variables believed to be associated with these types of stress corrosion. An ammonia stress-cracking apparatus similar in many respects to the one described has been assembled. Certain aspects of its construction may be of interest. Tensile loading of the specimens, which are usually Y8-in. diameter wires, is accomplished by springs acting in compression in compact, portable, tubular assemblies weighing less than 10 lb. The lower end of each assembly contains the test specimen and is passed into the test chamber for exposure to the moist ammoniacal atmosphere. There is considerable convenience in being able to load the specimens in a portable unit, which may be warmed to prevent condensation, and then thrust instantaneously into the test chamber. Spring loading obviates the use of weights, but it has the disadvantage of allowing some relaxation of the load if the specimen elongates during corrosion. The maximum loss in load found so far was 20 per cent. The air supplied to the test chamber is humidified by passing it through thermo¬statically controlled water. The air is dispersed into fine bubbles by being forced through a porous ceramic filter at the bottom of a tank containing about 10 liters of water. The temperature of the water is controlled independently of the tempera¬ture of the test chamber. Thus, with the

Jan 1, 1945

By Quentin Singewald

SOME of the broader relations between structure and ore deposition along the London fault, deduced from a thorough study of the geology of the eastern part of the Mosquito Range, should be of general interest to economic geologists. The first part of this paper is a generalized state-ment of the geology of the region in which the London fault is located; it may be supplemented by reference to several earlier publications by the writers and to the U. S. Geological Survey's Professional Paper 148, on the Leadville district. The second part deals with the structure of both the fault and the disturbed zone adjoining the fault. The third part dis-cusses the salient features of the ore deposits, particularly emphasizing structural control. The two generalized maps are complementary to one another but contain too many data to show on a single small map. The London fault is between Leadville and Alma, and the ore deposits along it are said to lie in the Alma district. Field work in this district, during six summers since 1927, has been a part of the cooperative work of the U. S. Geological Survey, the State of Colorado, and the Colorado Metal Mining Board. The writers have made use of work by R. D. Butler, J. W. Vanderwilt and R. E. Landon. G. F. Loughlin and C. H. Behre, Jr., who have worked on the west side of the range, have con-tributed valuable suggestions. Mining men of the district have aided in many ways.

Jan 1, 1936

By Merrill, Charles White

MOST extraordinary of the technical developments in placer gold mining during the last five years has been the rise of the dragline dredge, by which is meant a floating washing plant for auriferous gravel, fed by a dragline excavator. The idea originated in the fall of 1933, when Horace Onyett constructed a floating washing plant to which gravel was delivered by a dragline excavator standing on dry land. Onyett's operation near Oroville, Calif., and another started by H. F. England later on Wyandotte Creek, Butte County, Calif., yielded '75 oz. of fine gold before the end of 1933. Although the first operation was abandoned shortly as un- profitable, the dragline-dredge method of gold recovery soon began to expand at a boom rate. As a matter of interest, the Onyett operation was taken over later by Lord and Bishop, who are re- ported to have succeeded in making it the first financially successful drag- line dredge. In California alone drag- line dredges produced $3,294,970 worth of gold in 1937, and the pros-

Jan 1, 1938

Mining Methods LUCIEN EATON, Chairman GERALD F. SHERMAN, Vice-chairman CHARLES W. WRIGHT, Secretary Alluvial Mining CLINTON BERNARD CHARLES H. MUNRO CHARLES JANE N H. R. NORSWORTHY Open-cut Mining Iron MAX H. BARBER J. A. MacKILLICAN Copper MICHAEL CURLEY H. B. TEMPEST Underground Mining Iron C. H. BAXTER CARL BREWER TENNEY C. DESOLLAR Copper W. B. DALY A. H. WOHLRAB R. W. THOMAS

Jan 1, 1934

By T. J. Whalen, M. Humenik

The liquid surface tension of copper-nickel ad copper-nickel-titanium-carbon alloys and the wettability of titanium caybyde by these alloys have been measuhed. It was found that the surface tensions of the binary copper-nickel alloys Lie on a smooth curve between the end members, copper and nickel. The addition of small amounts of titanium and carbon has nO effect on the surface tensions of copper-nickel alloys. Small additions of nickel to copper significantly reduce the contact angle of Ike alloy with titanium carbide. From a Gibbs treatment, nickel is shown to be adsorbed at the titanium carbide-alloy interface. X HE microstructure of two-phase materials has been shown to be influenced largely by the interfacial energies between the phases present.' , In systems prepared by powder metallurgy techniques and densi-fied in the presence of liquid phase, a precise analysis of microstructure and interfacial energy relationships requires a knowledge of the solid-solid interface energies and liquid-solid interface energies. However, marly metal-nonmetal systems are characterized by the "sweating" of the liquid during sintering, and in these systems wettability is a principal consideration. The wetting in turn is dictated by the various interface energies of the system, as shown in Fig. 1 for a liquid drop formed on a solid substrate. The equation which expresses the vectorial balance of surface forces in the horizontal plane, at the point of contact, A, is given by: where ssv = solid-vapor interface energy sSL = solid-liquid interface energy sLV= liquid-vapor interface energy 6 = contact angle measured through the liquid phase. The angle and the surface tension, slv, can be measured accurately by the sessile drop method.3, The absolute value of the surface energy of the solid cannot be determined by this method, but with reasonable changes in the composition of the liquid only, the value of ssv can be considered constant. The changes in contact angle, then, can be attributed to changes in sSL and sLV and since sLV can be measured, the changes in sSL can be determined. Several studies have indicated that the surface and bulk properties of solid alloys can be correlated with electronic structure. The catalytic activity of copper-nickel alloys was reported to follow the dband vacancies in these alloys.5 Nickel has been considered to have 0.6 holes per atom in the d-band. The addition of copper to nickel is thought to bring about a filling of the d-band of nickel, since each copper atom contributes one electron. Thus, at an atomic concentration of 60 Cu-40 Ni (62 wt pct Cu-38 wt pct Ni) the d-band is believed to be full, and magnetic measurements support this view.6 If the electronic structure is influencing a property of the alloy, this property should show some sort of discontinuity as the composition changes from one side of the 60 Cu-40 Ni composition to the other. Since the catalytic activity can be considered as a surface property of the alloy, it is logical to assume that other surface properties, such as surface tension, may also be influenced by electronic structure. The suggestion has been made that there is a correlation between the solid titanium carbide-liquid Cu-Ni alloy interfacial energy and d-band filling.7 One purpose of this investigation was to determine if the changes taking place in the electronic structure with compositional changes in the solid copper-nickel alloys were reflected in the surface tension values of the liquid alloys. Such a change, if present, would lend support to the suggestion that one can refer to discrete energy bands in the liquid state. Other purposes of the present study were to investigate in detail the wettability in the system copper-nickel-titanium carbide, and to discuss the possible processes which take place during wetting in this system.

Jan 1, 1961

By Carle R. Hayward

The growing importance of metallography has caused a corresponding interest in the improvement of apparatus for preparing specimens of metals and alloys for microscopic examination. The purpose of this paper is to describe an electric heating-furnace, a grinding- and polishing-machine, and a device for mounting specimens, which are used in the metallographical work at the Massachusetts Institute of Technology. These three pieces of apparatus were designed and made in the laboratory of the Institute, and each possesses some original features which may be of interest. Electric Heating-Furnace. The accurate control of heat necessary for metallographic work is best obtained by the electric-resistance furnace. Uufortunately, however, even the platinum-wound furnaces cleteriorate with use and ultimately burn out, while the cheaper resistance-materials are often short-lived. Since the resistance-coil must be replaced from time to time, it is of advantage to be able to make this change with as little trouble as possible, and this is an important feature in the furnace shown in Fig. 1. A is a cylindrical galvanized-iron can, with two handles, B. A porcelain tube, C, passes through the central hole in the cover of the can and rests upon the asbestos disk, D; the bottom of the tube is held in place by the asbestos ring, 3. The space, F, around the tube is filled with powdered magnesia. G is an ordinary assay-crucible, with the cover inverted so as to present a smooth top for supporting a second porcelain tube, H. The latter is wound with " Excello " resistance-tape, 0.014

Jan 1, 1912

By R. A. Graham, R. W. Rohde

The effect of hydrostatic pressure upon the austenite start temperature of a commercial Fe-28.4 at. pct Ni-0.5 at. pct C alloy has been determined. For pressures to 20 kbar, the austenite start temperature decreased from its atmospheric pressure value of 380°C at the rate of about 4°C per kbar. These data are analyzed by two different thermodynamic approaches; first, considering the transformation as an isothermal process, and second, considering the transformation as an isentropic process. It was found that both these approaches fit the experimental data equally well. The effect of hydrostatic pressure upon the austenite start temperature is best described by considering the mechanical work done during the transformation as that work obtained by multiplying the applied pressure with the gross volume change of the transformation. It is widely recognized1 that strain has an important effect on the initiation of martensitic transformations.* For example, the martensite start tempera- *In this paper, use of the term martensitic transformation implies the reversal of martensite to austenite as wen as the formation of martensite from austenite. ture, M,, may be increased by plastic deformation. Similarly, plastic deformation is observed to lower the austenite start temperature, A,. The effect of uniaxial stress on the M, of iron-nickel alloys has been studied by Kulin, Cohen, and Averbach.2 They found that the martensite start temperature was significantly changed by stresses well within the elastic region. Moreover, the effect of tensile and compres-sive stresses differed. These effects were explained in terms of the interaction of the applied stress with both the dilational and shear components of the transformation strain. The magnitudes of the influence of uniaxial tension, compression and hydrostatic pressure on Ms were measured in 30 pct Ni 70 pct Fe by Pate1 and Cohen.3 Their thermodynamic calculations and similar calculations by Fisher and Turnbull4 predicted the experimental results when the transformation was assumed to occur isothermally at some fixed driving force. This driving force was assumed to be supplied by a combination of the chemical free energy difference between the austenitic and martensitic phases and the work performed during transformation by the applied stress. More recently, Russell and winchel15 reported the effect of rapidly applied shear stress on the reversal of martensite to austenite in iron-nickel-carbon alloys. They performed a thermodynamic analysis of this transformation based upon the assumption that the re- versal occurred adiabatically. They concluded that the applied shear stress did not significantly interact with the transformation strain and thus did not assist in inducing the reversal. Rather they concluded that the reversal was effected by localized strain heating which resulted from the gross local shear deformation of the experiment. In either the adiabatic or isothermal analysis it is necessary to compute the work performed by the interaction of the applied stress and the transformation strains. In the case of hydrostatic pressure this interaction has been treated by two different methods. In either case the applied pressure is assumed to remain constant during the transformation. In one treatment the applied pressure is assumed to interact directly with the dilatational strain associated with the formation of an individual martensite plate.3'4 This local strain has been measured at atmospheric pressure in iron-nickel alloys by Machlin and Cohen.6 In the above treatment this local strain is assumed invariant with temperature and pressure changes. In the other treatment the applied pressure is assumed to interact with the gross volume change of the transformation.7,8 The usefulness of this latter treatment has been demonstrated by Kaufman, Leyenaar, and Harvey7 who calculated the effects of pressure upon the martensite and austenite start temperatures of Fe-10 at. pct Ni and Fe-25 at. pct Ni alloys. Excellent agreement was obtained between their calculations and their experimental data on an Fe-9.5 at. pct Ni alloy. However, this treatment suffers from the fact that the data required to calculate the volume change of the transformation (i.e., the initial specific volumes, the thermal expansion and compressibility data for both the austenitic and martensitic phases) is, in general, not available for any material except pure iron. Thus the calculations of Kaufman et al.7 were necessarily performed by assuming that the volume change of the martensitic transformation in the iron-nickel alloys was that same volume change occurring during the a-? transformation in pure iron. While this approximation may suffice for very dilute alloys it is likely to be inaccurate in high nickel alloys. We have performed measurements of the effect of hydrostatic pressure to 20 kbar on the A, temperature of an Fe-28.4 at. pct Ni-0.5 at. pct C alloy. The composition is similar to the alloy used by Pate1 and Cohen3 to determine the effect of pressure upon the M, temperature. The present measurements permit calculation of the interaction between the applied pressure and the transformation strain. Additionally, measurements have been made which allow precise determination of the gross volume change of the transformation. The data allow direct comparison between the alternate hypotheses of the interaction between the applied pressure and a dilatational transformation strain characterized by either the formation

Jan 1, 1970

A tentative plan for the Colorado Meeting has been formulated as follows: One day will be spent at Denver, one day at Colorado Springs, one day at Cripple Creek, a trip by automobile to the top of Pike's Peak, one day at Pueblo, one day at Leadville. All the principal mines and mills of the districts mentioned will be visited, including the gold mines in Cripple Creek, the lead, zinc, and steel works. of Pueblo, the production of ferro-molybdenum by electric furnace at Leadville, etc. Special arrangements are being made for the social entertainment of ladies at all points; one evening at Colorado Springs will be devoted to a reception and dance, and the usual dinner will he given on another evening. The following papers have already been accepted for the Colorado Meeting, and some have already been published: Fireproofing Mine Shafts by the Anaconda Copper Mining Co. By E. M. Norris. (March Bulletin.) Air Blasts in the Kolar Gold Field, India. By E. S. Moore. (March Bulletin.) The Use of Coal in Pulverized Form. By H. R. Collins. (April Bulletin.) Coal Mining in Washington. By F. A. Hill. (April Bulletin.) Carbocoal. By C. T. Malcolmson. (May Bulletin.) Gaging and Storage of Oil in the Mid-continent Field. By O. U. Bradley. (March Bulletin.) An Interpretation of the So-called Paraffin Dirt of the Gulf Coast Oil Fields. By A. D. Brokaw. (April Bulletin.) The Theory of Volcanic Origin of Salt Domes. By. E. DeGolyer. (May Bulletin.)

Jan 5, 1918

By Arthur C. Spencer

IN extension of a suggestion already made to account for certain features observed in the Juneau gold-belt in southeastern Alaska,' it is the object of the present paper to indicate in detail certain conditions in which deformation of rocks under their own weight might lead to the production of fractures in which veins could be deposited. A direct, uniformly-distributed pressure of sufficient intensity applied to an elastic brittle mass offering strong resistance to deformation produces rupture. In a material of ideal properties the surfaces of rupture under such pressure would be shearing planes inclined at 45° to the line of force, unless there be preliminary deformation, in which case this angle would be greater than 45°. This general conclusion, resting upon ana¬lytical mechanics, is completely supported by the results obtained by Daubrée in experiments upon the deformation of wax and resin prisms under compression. Let us then first con¬sider one of Daubrée's diagrams. In the case illustrated in Fig. 1, four sets of fractures in two appproximately right-angled pairs (that is to say, in conjugate sets) were produced by end-wise compression of the square cross-sectioned prisms. These fractures cut the axis of compression at approximately equal angles, not varying greatly from 45°. The location of the four sets of fractures is obviously determined by the shape of the prism, since the material in each corner acts in a way as a buttress, permitting the bulging to take place most readily on the sides. By limiting the directions in which bulging may take place, results of a more simple nature could be obtained. Take, for instance, a square prism and place it between two fixed and

Nov 1, 1905