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By E. J. Dulis, G. V. Smith

AS reported several years ago,' nitrogen may be taken up from the atmosphere by austenitic Cr-Ni steels during creep or creep-rupture tests. This was indicated by chemical analysis and by the appearance of a new microstructural phase, or phases, tentatively identified as chromium nitride (S), at the surface or at the intergranular cracks associated with fracture. The nitrogen pickup was observed to be dependent on time, temperature, and deformation. In a more recent investigation, a sample was obtained in which there was sufficient of the precipitate to suggest that it could be readily identified by X-ray diffraction. This sample had been taken from a 1/4 in. diam creep-rupture specimen of annealed, type 304L stainless steel of the following initial composition: C, 0.03 pct; Mn, 0.65; P, 0.010; S, 0.019; Si, 0.54; Cr, 19.50; Ni, 12.02; N, 0.031; and Al, 0.005. The specimen had ruptured after 10,470 hr at 1500°F (2000 psi). In this case nitrides were distributed across the whole section of the sample, Fig. 1. The precipitate occurred both at the grain boundaries and within the grains; the latter precipitate had in some cases the appearance of pearl-ite, and in others was distinctly Widmanstatten. Chemical analysis of the sample after test showed 0.64 pct "soluble" nitrogen (soluble in 1:1 hydrochloric acid: water) and 0.18 pct "insoluble7' nitrogen (insoluble in the hydrochloric acid solution but dissolved by fuming sulphuric acid). For identification of the precipitate by X-ray diffraction, the matrix in the surface layer of the specimen was dissolved by prolonged attack in an alcoholic solution of picric and hydrochloric acids. The appearance of the specimen surface after such etching is shown in Fig. 1c. The diffraction pattern of the surface-concentrated precipitate was obtained with a recording spectrometer in both the forward and back-reflection regions (the latter by adapting a special fixture to the conventional X-ray unit). The observed X-ray diffraction lines, Table I, show the presence of Cr,N and CrN; the agreement with interplanar spacings calculated from reported data2,3 is quite good. Since it has been suggested' that CrN dissolves only in concentrated sulphuric acid, whereas Cr2N dissolves in dilute hydrochloric or sulphuric acids, an effort was made to distinguish between the two nitrides. This proved possible, inasmuch as etching in a dilute solution of hydrochloric acid gave a sample in which microscopic examination showed that much of the Widmanstatten-pearlitic precipitate within the grains had been eaten out, leaving the grain boundary precipitate in relief, and which, when examined by X-ray diffrac-

Jan 1, 1953

By J. S. Kasper, R. M. Waterstrat, B. F. Decker

THE existence of v phase in the Mn-Mo system was discovered in this laboratory several years ago,' but neither the conditions of its formation nor its composition were known, and preliminary attempts to reproduce the phase were unsuccessful. We wish now to specify the information appropriate to phase formation on the basis of experiments performed since that time. The starting materials were in every case electrolytic manganese and high purity molybdenum. Two methods of preparation were employed: l—arc-melting varying combinations of the elements in an inert atmosphere and subsequent heat treating, and 2—sintering compressed mixtures of finely divided powders of the elements. In the latter method, the powders were first passed through 200 mesh screen and then compressed into cylinders of % in. diameter and % in. length, which were sintered at elevated temperatures in an atmosphere of dry hydrogen. For some samples, the sintering temperature was 1200°C (for 1 hr), and these were then heat- treated at lower temperatures for times up to 24 hr. Eventually it was found, for the proper composition, that essentially pure a phase could be produced by sintering at 1125°C for 3 hr. Quenching to room temperature was effected by means of a stream of cold, dry hydrogen in a water-cooled chamber. The arc-melting procedure was found to be unsatisfactory after an investigation of many samples at different compositions and temperatures. Large quantities of manganese were vaporized during melting and none of the products were homogeneous or contained extended regions of pure phase. Nonetheless, these experiments established that no formation occurs in the Mn-Mo system below 1115oC, and indicated, at least roughly, the composition range of interest for further exploration. The more definite results obtained from samples produced by the second method are given in Table I. A portion of sample 2 heated for 16 hr at 1000°C in a Vycor tube transformed to molybdenum plus unidentified phases of complex X-ray pattern. From these few results it appears that the region of phase is quite narrow in composition. It is of interest that the composition is such as to make for difficulties in correlating this structure on an electron atom basis with other a structures of iron, cobalt, and nickel. In that respect Mn-Mo shows the same anomaly as Mn-Cr and Mn-V systems.' A second feature is that in common with the two other known molybdenum (Fe-Mo and Co-Mo), Mn-Mo v exists only at elevated temperatures. The X-ray powder pattern of the pure a phase of Mn-Mo is given in Table 11. It agrees well with the patterns established for other structures, especially with that for Fe-Mo as given by Goldschmidt.An attempt is being made to establish whether an ordering of the respective atoms occurs and such information will be reported in a future publication. Acknowledgment The authors acknowledge gratefully the assistance of Mrs. J. R. Belanger in some portions of this work. References 'J. S. Kasper, B. F. Decker, and J. R. Belanger: Journal of Applied Physics (1951) 22, p. 361. 2 A. H. Sully: Journal Inst. Metals (1951) 80, p. 173. H. J. Goldschmidt: Research (1949) 2, p. 343.

Jan 1, 1954

By Carl A. Zapffee

FOR a number of years a puzzling phenomenon of brittleness in Class II ferritic stainless steels, developing in the temperature range near 475C, has received increasing attention, but its nature remains essentially unknown. During an investigation of the fractographic structures in stainless steels, conducted in the author's laboratory the past several years, principally under sponsorship of the Office of Naval Research, some observations of a new kind were found for "475 °C embrittlement." While the details of the study cannot be given here,' three fractographs will suffice to carry the

Jan 1, 1952

By L. F. Stutzman, George Thodos

A new graphical method, which is a modification of that proposed by Buckley and Leverett', is presented for the determination of the displacing fluid saturation at breakthrough for frontal drive mechanisms. This method is applicable to all types of fluids, which may be either soluble or insoluble in the oil at reservoir and injection conditions. This adaptation has unique advantages in handling problems in which either liquids or gases are the displacing fluids. INTRODUCTION In the displacement of oil from a reservoir with water or gas injected into the formation or by the expansion of a gas cap, the determination of breakthrough or flood advance is important to define the initial and subordinate phases of the operation. Thus, the determination of the displacing fluid saturation at breakthrough is fundamental to the establishment of over-all reservoir production. Methods for analyzing this saturation and for calculating production rates have been previously reported1,'*".". All of these methods utilize the rate equation for linear flow developed by Buckley and Leverett1. xs = QT - Qn/A? (?fu/?Su) .....(1) Sp where f, represents the volumetric fraction of displacing fluid in the total flowing fluid within the reservoir as is defined by: fo = 1/1+ ku/kd µn/µn .......(2) Since the time, ?, necessary for the flood front to travel distance ?X is unknown, Eq. 1 cannot be solved directly for the determination of the breakthrough point. Therefore, it becomes necessary to solve Eq. 1 simultaneously with an equation representing a fluid bal-ance on the reservoir behind the flood front. To develop such a fluid balance equation, it has been assumed that the fluid composition is uniform in the reservoir behind the flood front. Based upon this assumption, the follow-ing equation can be derived from a material balance on the displacing fluid: x = (?X) s Dx ? x=0 [ Snx - Sn1 ] dx = QT - Qn/A? It is readily observed that the displacing fluid satura-tion behind the flood front, Snx, may be determined through the simultaneous application of Eqs. 1 and 3. Although the approach may vary, this objective re-mains the same for all of the previously mentioned graphical or analytical methods. After Sox is determined, it is then possible to calculate the gas-oil and/or water-oil ratios and the rates during the initial and subordinate phases of production, and thereby define the production history of the reservoir. In this presentation only the de-termination of Snx is considered, and the reader is re-ferred to the several texts in reservoir engineering2,4,5 for a complete discussion on the methods for establish-ing the production history of a reservoir. PROPOSED METHOD FOR DETERMINING Snx Since at any time the quantity, QT - Qn/A? is a constant, Eq. 1 may be expressed in differential form as follows: dxsn = QT - Qn/A? d (? fn/? Sn) sn .....(4) Eq. 4 may be substituted directly into Eq. 3 to obtain: ? fn/? Sn ? [ Snz - Sn] QT - Qn/A? d ( ? fn/? Sn) = QT - Qn/A? ...............(5) Eq. 5 simplifies to the expression: ? fn/? Sn ? [ Snz - Sn] QT - Qn/A? d ( ? fn/? Sn) = 1 ....(6)

Jan 1, 1958

By S. R. B. Cooke, C. E. Thurston, G. Kudo

The trend toward utilization of low grade iron ores means that more efficient methods must be developed for their concentration. The collecting ability of fatty acids derived from fish oils has been extensively investigated by Cooke.' Tuna oil, a byproduct of the tuna canning industry, is one of the lower priced fish oils. Utilization of tuna oil fatty acids as collectors in the flotation of iron ore might be economically feasible under certain market conditions, especially if their efficiency were high. Crude or unfractionated tuna oil fatty acids, and five fractions derived therefrom, were tested for their ability to concentrate a commercial specularite ore from northern Michigan. A commercial fatty acid derived from tall oil, and commonly used in nonsulfide flotation, was used as a reference. The crude fatty acids were obtained by simple saponification of tuna oil. Fractions A and B were obtained by acetone precipitation of the crude acids at -5O and -2S°C, respectively. Fraction C was obtained by a partial fractional distillation at 12S°C and at a pressure of 3y in a centrifugal molecular still in order to remove the shortest and longest chain fatty acids of tuna oil as well as oxidation products present in the original mixture. Fractions D and E were prepared by a chilling process in order to precipitate the unwanted saturated fatty acids. Yields and iodine values of the materials used are listed below: The seven samples were used as collectors in a laboratory procedure patterned after the commercial process for flotation of Michigan specularite ore. The outline of the procedure is that previously described1

Jan 1, 1962

By C. W. Schultz, R. B. Tippin

Statistical screening is so named because a particulate feed is separated into "size" intervals on the basis of the probabalistic behavior of the individual particles (i.e., their probability of passing the screen) rather than by physical restraint. To illustrate this statement, consider a conventional screening operation. A particle which is larger than the openings in the screen cloth is physically restrained from passing through and is repeatedly reflected from the surface until it is discharged as oversize. Of those particles smaller than the screen openings, the very smallest tend to pass the screen near the feed end while those nearer in size to the screen opening tend to pass at a greater distance from the feed end. Alternatively, we could say that the particles with high probability of passing through the screen are concentrated near the feed end while particles of low probability of passing are dispersed from the feed end. This tendency to segregate is the basis for size separation by statistical screening. The purpose of this note is to: 1) Show that the distribution of material passing an array of screens can be described by a modified binomial distribution. 2) Demonstrate that an efficient size separation can be made by this technique. 3) Relate some of the more important screening parameters to the efficiency of the size separation. The Distribution Function The distribution of undersize products along the length of a screen can be derived with the help of a few simple definitions and assumptions. 1) First, we must assume that each particle has some probability of passing a screen on a single presentation. Further, we must assume that this probability is constant and is not affected by the position of the particle on the screen. It must also be acknowledged that several factors enter into this probability. Among them are the "action" of the screen, the slope of the deck, the shape of the openings, etc. The relationship between these factors, however. is not the subject of this paper. 2) To simplify calculations, all particles falling within a size range on the Tyler scale, e.g., —x + x/ mm, are assumed to have the same probability. 3) It is assumed that particles which do not pass the screen on a presentation are reflected a unit distance forward, i.e., the direction of material travel. A unit distance is defined as the distance between the centers of consecutive wires in the screen cloth.

Jan 1, 1971

By W. Vickers

SALKOVITZ1 has given a number of useful angles between planes for use with the Laue method in determining the orientation of bismuth single crystals. Bismuth is usually considered as having a face-centered-rhombohedra1 structure with its axial angle 87°34', Fig. 1. A similar figure given by Sal-kovitz appears to be in error in that the angle there marked as 87°34' should be 92°26. The primitive cell is a single rhombohedron of axial angle 570 14. The structure is almost face-centered-cubic and hence high accuracy in measurements is essential if there is to be no confusion in indexing poles or zone axes. It is easier to get this accuracy if zone axes are plotted on the stereogram because they will lie near the basic circle where the net has a more open scale. The zone axes can be read from the film, using a Greninger chart, and can be plotted more accurately than poles. Also, the angles between points near the basic circle can be read more accurately than those between poles near the center. In order to use the zone axes the angles between directions have been calculated from a formula given by Niggli,2 and are given in Table I. Miller indices

Jan 1, 1958

By W. J. West, T. D. Mueller, J. E. Warren

The authors have presented valuable information on the influence of the interfacial tension and the contact angle on the recovery efficiency of the waterdrive process. It is considered, however, that the following points deserve a closer examination. 1. As pointed out by Wyllie and Spangler1 the displacement pressure PD i.e. the pressure required to initiate the displacement of the wetting phase from the core, is a measure of the maximum pore diameter dmax. If the capillary pressure Pe as a function of the wetting

Jan 1, 1956

By J. T. Richards

ELASTIC constants, including E-modulus, G-modulus, Poisson's ratio, and compressibility, are affected by temperature, but not necessarily to the same degree nor in the same direction. Theoretical expressions relating the temperature coefficients for the various elastic constants have been introduced by Gruneisen. In considering the thermoelastic characteristics

Jan 1, 1955

By Paul F. Fulton, Robert K. Estes

INTRODUCTION Relative permeabilities are factual data necessary to any prediction of reservoir production behavior. One important problem in determining relative permeabilities of porous media to gas is the effect of gas slippage on these determinations. Since certain aspects of the slippage phenomenon still remain unknown, this study is particularly concerned with that problem. The validity of the theory of gas slippage as it is applied to the flow of gas through porous media has been well established. 1,2,3 Therefore, in determining the permeabilities of porous media to gas by ordinary laboratory procedure, i.e., at atmospheric pressure, the slippage correction should be considered. Rose3 performed experiments on gas relative permeabilities which indicated that the effect of gas slippage on the measured effective gas permeabilities at various liquid saturations decreased with an increase in liquid saturation. Following Rose, it was substantiated experimentally' that the effective gas permeabilities at the various liquid saturations extrapolated to infinite mean pressure were the same as the non-wetting liquid permeabilities at the same saturations. This same paper also presented data which showed that the magnitude of the slippage between those values of gas effective permeability determined at atmospheric pressure and those found by extrapolation to infinite mean pressure decreased with an increase in liquid saturation. However, these experiments were not performed at liquid saturations above 30 per cent. Therefore, the purpose of this experimental work was to determine the effect of gas slippage on permeability measurements at liquid saturations in excesh of 30 per cent. APPARATUS Five core samples were used In this work: two synthetic Alundum samples (A-1, and A-2). a Nichols Buff sandstone sample (NB-13), and two samples from producing formations, a Soso sandstone (S-1), and a vugu-lar dolomitic limestone (R-7). The core samples ranged in permeability from 32 to 663 md. These cores were chosen because they represented a fairly wide range of permeabilities and probably a considerable difference in pore size and pore size distribution. Fig. 1 is a schematic diagram of the apparatus which consists of an air dehydration filter A, two Moore null-matic sub-pressure regulators B and C, the differential oil manometer D, the core holder E, the flowmeter F, the soap reservoir G, and a mercury manometer H measuring the downstream pressure. The interesting features of the apparatus are the two Moore vacuum-pressure regulators. The regulators permit the rapid establishment and easy control during flow at sub-atmospheric pressures of both the differential and downstream pressures, and prevent the surging action of the vacuum pump from disturbing the system during flow. Provided there are no leaks in the system, these regulators will maintain without measurable change selected downstream and differential pressure. Specifically, regulator B controls the downstream pressure and regulator C controls the differential pressure. In opera-

Jan 1, 1957

By W. E. Hall

The Darwin mining district of California, 160 miles north of Los Angeles, has yielded an estimated $45 million in lead, silver, zinc, and copper since 1875. The deposits are in silicated limestone of Penn-sylvanian and Permian age close to a stock of horn-blende-biotite-quartz monzonite. Steep left-lateral strike-slip faults that strike N 50o 70o E served as feeder channels for the ore solutions, and minor folds, favorable beds, and faults close to the feeder channels localized the orebodies. The orebodies are irregular, steep, pipe-like replacements that cut across bedding, bedding replacements, and fissure fillings in a calc-silicate country rock consisting mainly of wollastonite, grossularite-andradite garnet, idocrase, and diop-side. Near surface the ore consists of a soft, crumbly mass of cerussite, hemimorphite, jarosite, limonite, and some secondary copper minerals. The primary ore consists of galena, sphalerite, pyrite, pyrrhotite, and chalcopyrite with smaller amounts of andorite, matildite, scheelite, tetrahedrite, and a high silver-lead-bismuth-selenium-bearing galena. Preliminary X-ray fluorescence study of the primary ore has indicated unusually high concentrations of bismuth, selenium, and silver in galena from certain parts of the mine. One phase of this study concerns the distribution of these elements. Twenty-two samples of galena and thirty of sphal- erite have been purified and analyzed or are being analyzed. The selenium in 21 samples of galena ranges from 0.0045 to 2.11 pct; four contain more than 1 pct. These four samples were collected from the Essex orebody, where most of the selenium is concentrated. Three are from high-grade, near-surface ore, and one is from the 700 level. Four of the seven analyzed galena samples from the Thompson workings immediately north of the Essex orebody contain 0.29 to 0.74 pct Se; the others show less than 0.05 pct. Galena from the Defiance workings about 2000 ft south of the Essex has less than 0.03 pct Se. The selenium-bearing galena also contains concentrations of bismuth and silver. Preliminary spectographic analyses indicate as much as 3 pct Bi and more than 1 pct Ag in galena with high selenium content. Antimony is the only other minor element present in galena in amounts greater than 0.02 pct; most galena contains between 0.1 and 0.2 pct and the maximum is 0.72 pct. A second phase of the study is an attempt to determine the temperature range of the formation of the ore. The iron content of sphalerite deposited in equilibrium with pyrrhotite is being used as a geologic thermometer as it is a function of the temperature of deposition of the ore.' Preliminary results indicate temperature range from 430°C in replacement orebodies in the Defiance workings to 180°C in shallow fissure fillings.

Jan 1, 1960

By George F. Sowers

THE geophysical methods of exploration employed so extensively in mining and petroleum investigations are now being used in civil engineering. Requirements differ from those of mineral ex- ploration and therefore modified techniques have been developed. The civil engineer is primarily interested in the uppermost soil and rock strata. In highway engineering the materials affecting design and construction may be found within 15 or 20 ft of ground surface, and data on soils and rocks is seldom needed for more than a depth of 100 ft even for the heaviest structures.

Jan 1, 1954

By Harry Udin

IN 1948, the writer and his associates determined the surface tension of solid copper by balancing the force of surface tension in a very fine wire against an external load.' At that time we, in common with other early workers, assumed that grain boundary energy in a pure metal is very small in comparison to the energy of an external surface. Accordingly, we neglected the internal surface energy of the coarse-grained specimens. Since that time, experimental evidence has accumulated showing that grain boundary energy, far from being small, is generally about one-third of the energy of an external surface.2-4 This is sufficient to introduce a significant error into our determination. The differential equation governing equilibrium is: wdl - yds, + y*ds2 [I] rather than wdl = yds as originally written. w is the balancing force in dynes, 1 the length of the specimen, sl the external and s2, the internal surface area, y the copper/ copper vapor surface tension, and y* the grain boundary tension. Fortunately, we had made for another purpose a careful study of the size and shape of the grains, and found that the boundaries, with rare exceptions, traversed the specimens and were perpendicular to the wire axis. For this case, eq 1 leads to w = rry -(n) r2y* [2] where r is the wire radius and (n is the number of grains per unit length. A count of some twenty 5-mil wires indicated that - n became 80 & 10 after a short anneal near the melting point, and remained nearly constant for as long as 96 hr at temperature. An assumption of y* = 1/3y leads to a defining eauation for r: [31 The term in the brackets may be considered a correction factor applied to eq 11 of ref. 1. Upon applying this factor, the surface tension of solid copper at its melting point is found to be 1650 & 100 dynes per cm, rather than 1370 as previously reported.' The new temperature coefficient is —0.55 dynes per cm per "C. Grain boundary energy is more significant than surface energy to the physical metallurgist. It is evident from eq 2 that a series of experiments with wires of different grain size can lead to an evaluation of y*. The details of such an experiment are being worked out now. References 1 H. Udin, A. J. Shaler, and J. Wulff: The Surface Tension of Solid Copper. Trans. AIME, 185, 186-190; Journal of Metals (Feb. 1949) TP 25303. 2 G. L. C. Bailey and H. C. Watkins: Surface Energies in the System Solid Copper-Molten Lead. Proceedings Physical Society. (London) (1950) 36B, 350. 3 L. H. VanVlack: Inter granular Energy of Iron and Some Iron Alloys. Ph.D. Dissertation, Univ. of Chicago, Sept. 1950. 4 . P. Greenough: Grain Boundary Energies in Silver. R.A.E. Report, No. Met. 52. (May 1950) Fan-borough, Hants, England.

Jan 1, 1952

By J. W. Spretnak, R. Speiser

IT has been suggested that boron in steel may form a film entirely around the austenite grain and that this film is responsible for the boron hardenability effect. In this connection, it is of interest to examine some of the ramifications of the concentration range of boron usually employed in hardenable steels, namely 0.0005 to 0.003 pct in a grain size range of ASTM grain size No. 1 through No. 10. The ratio of the iron to boron atoms and the number of unit cells of y iron per boron atom are listed in Table I. Even at the highest concentration considered, there are 1600 unit cells of y iron per boron atom, assuming a uniform distribution of boron. To investigate the possibility of the boron film formation, the number of boron atoms required to cover the grain surface completely must be calculated. With some transition elements, boron crystallizes in sheets composed of equilateral hexagons very much like graphite.' The selected value for the length of a side is 1.80Å. A simple calculation shows that two boron atoms cover an area of 8.4x l0 -16 sq cm. Table II lists the number of atoms of boron required for the formation of the monatomic film and Table III lists the number of boron atoms per grain. The hypothetical cases of 100 pct and 10 pct adsorption are calculated (all boron atoms in a grain and 10 pct of all boron atoms in a grain are located at the grain surface respectively). In Table 111, all combinations of grain size and composition below and to the left of the solid line (100 pct adsorption) and the dashed line (10 pct adsorption) are excluded as to the possibility of covering the grain surface with a continuous boron film. Thus, even for 100 pct adsorption, the smaller grains can form the film only at the higher concentrations. For the best case, grain size No. 1 and 0.0030 pct B, the required degree of adsorption is 3.9 pct. The above calculations deal only with the number of boron atoms required to form a monatomic film and do not take into account the mechanism of concentration of boron at the grain surface and the possible limitations to the extent of this concentration at a constant temperature, as for example in the austenitizing process. The question next arises as to how this surface concentration can occur during an isothermal treatment. Such surface enrichment of boron must occur through the phenomenon of surface adsorption, i.e., the concentration of solute atoms in solid solution in the vicinity of the surface without precipitation. A solute atom will tend to concentrate at the grain boundary if it reduces the interfacial tension. The possibility of adsorption effects involving both boron and carbon in iron has been discussed.' In general, the tendency for a sol-

Jan 1, 1954

By W. E. Bron, E. S. Machlin

GRAIN boundary migration in V-shaped thin specimens of high purity silver was studied. Each specimen contained two crystals having the relative orientation: (111)A/(111)B; (ll0)A/(101)B. The boundary between these two crystals varied between a continuous curved and an alternating two plane interface. The plane interfaces were oriented parallel to (101)A/(011B) and (121)A/(211)B. Traces of these planes are shown in Fig. 1. Evidently the two plane interface, although of higher area, comprises lower total interface energy than the average curved boundary it replaced. The plane boundaries were found to move at 650 °C to consume the broad segment of the V opposite to the direction of interface area and energy decrease. On investigation, using the thermal etching technique of Hendrickson and Machlin,1 it was found that the outer grain contained 8.3x108 more dislocations per cm" than the grain at the apex of the V. Consequently, the boundary moved to decrease the strain energy associated with the difference in dislocation density across the boundary. The rates of motion of specific {110} and {112} boundaries were measured during interrupted anneals at 650°C by referring the position of the boundaries to each other and a fiducial line on the specimen surface. The measured rates of motion are 0.075 and 0.025 mm per hr for the {110} and {112} boundaries, respectively. Plots of grain boundary motion vs time of annealing show straight lines with little deviation of data points from these lines.

Jan 1, 1957

By P. R. Sperry, P. A. Beck, J. Towers

Dahl and Pawlek1 found that electrolytic copper develops extremely coarse grains at 1000°C after about 90 pct reduction by rolling. This coarsening occurs only under conditions of penultimate grain size, deformation, and alloying which lead to the "cube" recrystallization texture.l,2,3,5 The peculiar angular shapes and straight grain boundaries of the coarse grains were noted by several investigator.1,4,5 On the other hand, coarsening in Fe-containing aluminum or in AI-Mn alloys8 does not depend on a "cube" (or any well developed) recrystallization texture. It is true that increasing deformation by rolling, and, therefore, an increasingly well developed re-crystallization texture, are associated with decreasing incubation periods of coarsening.6-7-8 Nevertheless, coarsening readily develops in aluminum even after only 30 pct reduction by rolling, where the recrystallization texture is very weak.6,8 Also, coarsening was observed by Jeffries9 many years ago in sintered thoriated tungsten, which presumably has no preferred orientation. In all these cases coarsening is associated with grain growth inhibition by a dispersed second phase.8,9 The annealing temperature has to be suficiently high to overcome the inhibition at a few locations. But if it is too high, growth starts at many points, and the resulting grain size becomes much smaller.9 Normally, the coarse grains are more or less equiaxed, and the boundaries have a typical ragged appearance.6.8 Cook and Macquarie4 demonstrated that, in addition to the texture-dependent coarsening previously found at 1000°C,l electrolytic tough pitch copper may also coarsen at 800°C after 50 pct reduction by cross rolling. The coarse grains formed under such conditions have rounded shapes and ragged boundaries, like those in aluminum. When the annealing temperature is higher, the tendency for their formation decreases. All these observations suggest that the coarsening at 800°C is associated with inhibition by a second phase. Actually, coarsening at 800°C after 50 pct reduction by cross rolling was observed only in tough pitch copper,4 which contains Cu2O particles. On the other hand, the texture-dependent 1000°C coarsening occurs in both tough pitch and oxygen-free copper;4 it does not appear to depend on the presence of a dispersed second phase. However, the interpretation of the 800°C coarsening in Cu after 50 pct rolling as an inhibition-dependent process, similar to the coarsening in A1-Mn alloys, is somewhat weakened by the fact that this coarsening was reported4 to occur only after cross rolling, and not after straight rolling. It was, therefore, decided to re-examine this question. A 1 in. diam electrolytic tough pitch copper rod, No. 2 hard drawn, was annealed for 20 min at 700°C, rolled to 0.5 in., annealed 10 min at 700°C, and straight rolled to 0.064 in. It was then given a penultimate anneal of 20 min at 500°C and it was cut into four sections, which were given final reductions by straight rolling as follows: A 30 pct reduction of area B 50 pct reduction of area C 70 pct reduction of area D 90 pct reduction of area Specimens cut from the four sections were finally annealed at 800°C in an oxidizing atmosphere. Strip A remained fine grained up to 10 hr, but the specimen annealed 12 hr consisted of only 2 large grains. Strip B had a few scattered large (1/2 to 3/4 mm) grains after 1 min, although the balance of the specimen consisted of fine grains of about 0.02 mm. After 5 min there were several 10 to 15 mm grains present, and after 1 hr strip B was completely coarsened. The coarse grains had the same characteristics (see Fig 1) as those obtained by Cook and Macquarie at 800°C after cross rolling. Strip C had several grains of 0.05 to 1 mm after 1 min, but it was still largely fine grained after 12 hr. After 48 hr it consisted entirely of grains of about 0.5 to 4 mm, with an extraordinarily large number of twin bands. Strip D remained com- pletely fine grained after 4 hr at 800°C. These results indicate that, in the deformation range of 30 to 70 pct reduction, the incubation period for coarsening as well as the rate of growth and the final size of the coarse grains decreases with increasing deformation. Similar

Jan 1, 1950

By A. E. Nehrenberg

IN an earlier publication' it was shown that the.. shape assumed by a volume of growing austenite is inherited from the prior structure. The matrix grains of pearlitic microstructures are equiaxed, and austenite grows in an equiaxed manner in these prior structures. Martensite and bainite, on the other hand, have an acicular grain structure, and the austenite produced in such structures grows in an acicular manner. In the discussion of this paper' it was pointed out that in cold-rolled tempered martensite, austenite grows in an equiaxed, rather than an acicular manner. The results of an experiment carried out to arrive at an understanding of this behavior are illustrated by the micrographs. Fig. 1 shows the acicular microstructure produced by heating tempered martensite to a temperature within the Ac1-Ac3 range, 1350°F. When tempered martensite is cold rolled, then heated to the same temperature, the equiaxed structure shown in Fig. 2 is produced. A sample of cold-rolled tempered martensite heated at 1350°F just long enough for the formation of a small amount of austenite is shown by Fig. 3 to have an equiaxed (recrystallized) ferrite grain structure. The small particles of. austenite which formed at 1350°F in the equiaxed ferrite matrix are likewise equiaxed. Thus, the equiaxed growth of austenite in cold-worked tempered martensite is not a contradiction of the principles described in the previous paper, for the growth pattern reflects the matrix grain structure existing at the time of austenite formation. References A. E. Nehrenberg: The Growth of Austenite as Related to Prior structure. Trans. AIME (1950) 188, pp. 162-174; Journal of Metals (January 1950). 2 J. R. Vilella and R. A. Grange: Discussion of ref. 1. Trans. AIME (1950) 188, pp. 1378-1381; Journal of Metals (November 1950).

Jan 1, 1953

By R. C. Hall

DEVELOPED to grow single crystals of alloys of high hardness and high melting points is a simple but effective apparatus described in this note. Growth from the melt, that is, by the Bridgman technique, hay be applied to metals or alloys which are physically hard as long as no phase transformation occurs on cooling to room temperature. The present apparatus was employed to grow single crystals of the ferromagnetic AI-Fe alloys above 1 wt pct Al and the Si-Fe alloys above 3 wt pct Si. Single Crystal Growth In a simple form, the method for growth of single crystals from the melt requires a molten metal charge in a pointed crucible which is slowly low-ered through a heated zone into a colder zone. Solidification starts at the bottom point and continues up the charge as the crucible is lowered through the heated zone. If a single crystal nucleates at the bottom, one crystal may grow throughout the charge under ideal conditions of slow growth.4,5 The presently developed method of growth was designed so that the chances that more than one crystal would grow were small. The single crystals were growth by the apparatus illustrated in Fig. 1. The charge was in the form

Jan 1, 1958

By G. P. Chatterjee

HARDNESS is one of the most common properties of metals and alloys but is one of the most difficult to define or express in terms of the fundamental units. In the Brinell or Vicker's hardness test, the hardness number N is defined as N = L/A where L is the load in kilograms and A is the area in mm'. This does not necessarily imply that a pressure of N kilograms per mm2 actually acts on the specimen.' It is essential that for a true comparison of hardness values the angle of indentation be kept constant,' a which is not done in the Brinell test. For this and other reasons, the Brinell hardness value is not based on a satisfactory physical concept.' The concept of hardness based on the work done per unit volume of indentation3-6 offers a simple and scientific definition. An attempt has been made here to develop this concept (at constant angle) and to compare the values so obtained with the Bhn for different metals and alloys. In Fig. 1 a vertical load L is applied to a compara- tively hard ball of diameter D creating an indentation of diameter 6 and depth h on the specimen S. The work done, W, is then given by W = So Ldh. [I] Since L is not independent of h, Honda and Takahasip and Matsumura" assumed different functions leading to equations which do not apply equallye to a wide variety of metals and alloys. A better relation is obtained from Meyer's Law L = ad" [2] where A and n are constants depending on the nature of the material but independent of the ball diameter D. From Fig. 1 it is obvious that h = R(l — cosq) and d = 2R sin 8.

Jan 1, 1957

By R. W. Heins, N. Street

Recently Hiller1 reported results on the impairment of the strength of quartz glass rods through wetting, indicating that there was general agreement with the prediction of the Griffith formula in that for the liquids used the rods were weakest in water i.e. the liquid which probably had the greatest free energy of immersion. The Griffith equation predicts that the tensile stress necessary to propagate a crack of length c is where ? is the interfacial free energy, E Young's modulus. Since for a solid immersed in a liquid of surface tension ?L and contact angle 8 at the solid-liquid-gas contact, ?s - ?SL = ?L cos ? where ?s is the surface free energy of the solid. Hence comparison between ?L cos 0 and strength impairment should be possible. In a study of the usefulness of the Kuznetsov pendulum2 as a means of studying rock drillability we have determined the effects of various liquids on the pendulum hardness of Bavarian limestone. The pendulum used had diamond points (Burgess Vibro-graver), a period of 1.14 sec and a total on sample weight of 1191 g. The decline of the pendulum oscillations was recorded by a light beam on light sensitive paper carried on a kymograph. Rehbinder's expression relating hardness to amplitude attenuation as a function of time can be written In A = - (1/H) t + In Ao where A, A, = amplitude at time t and initial amplitude respectively, H = hardness parameter, and t = time. The line of best fit to the experimental points was determined using the IBM 7090 electronic computer, the computer also gave A, by extrapolation to zero time. The results for the various liquids tested are given in Table I and Fig. 1. The limestone surfaces were highly polished before testing and each reported hardness value represents the average of at least ten separate determinations of the pendulum decline curve. On each newly prepared surface the water value was again determined (also

Jan 1, 1964