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By Samuel D. Warriner

(Wilkes-Barre Meeting, June, 1911.) THE dealings between concentrated capital invested in the conduct of our various industries and the combinations of labor known as "trade union organizations," have produced not only in the United States, but abroad, many novel methods of negotiation between employers and wage-workers. The size and strength of these organizations have destroyed the personal elements formerly governing the dealings between employer and employee and have produced various forms of trade-agreements now in more or less successful operation. The difficulty, however, has- been to secure consent of both parties to an equitable agreement. For this purpose there have been devised various forms of arbitration, either compulsory under the shadow of governmental legislation, or voluntary by mutual agreement. But these have not been altogether successful from a technical stand-point, for the reason that a compromise has generally been necessary, and in an effort to reach an agreement, terms have been made which have been neither fair nor satisfactory to either of the contending parties. The Anthracite Board of Conciliation represents one of the few thoroughly successful courts for the settlement of trade-disputes, if not the only one which has yet been evolved. The prestige of this board rests upon its successful treatment of the labor-troubles of the anthracite region for a period of more than eight years, and upon the fact that it has been able not only to reach decisions based upon the merits of the controversies, but to enforce its decisions upon both the employees and the employers. It has never been obliged to shape its conduct to secure the consent of the contending parties, and its decisions have been strictly and, in the main, cheerfully observed. The remarkable feature of this board has been that it has

Aug 1, 1911

THOSE NOT MARKED ARE MEMBERS; MARKED THUS t ARE ASSOCIATES. HEAVY-FACED TYPE SIGNIFIES HONORARY MEMBERSHIP. JUNIOR MEMBERS ARE MARKED II. THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION. AARONS, J. BOYD, Genl. Mgr., Chaffers G. M. Co., Boulder City, West. Australia. '05 ABADIE, EMILE R., Min. Engr Box 291, Porterville, Tulare Co., Cal. '76 ABBOTT, CLARENCE E., Genl. Supt., Iron Mines Div., 1405 Minnesota Ave., Bessemer, Ala. '04 ABBOTT, J. W., Min. Engr., "St. Omer," 123 N. Grand Ave., Los Angeles, Cal. '94 ABBOTT, Louis BENJAMIN, Chief Engr., Consolidation Coal Co., Elkhorn Div., Jenkins, Ky. '15 ABBOTT, ROBERT R., Met. Engr., Peerless Motor Car Co., Cleveland, Ohio. '12 ABE, ASAKA Yamagano G. M., Satsuma-Gori, Satsuma, Japan. '14 || ABRAHAMS, A. I., Student 1391 Madison Ave., New York, N. Y. '14 tACKER, E. O'C., Met Bethlehem Steel Co., Bethlehem, Pa. '86 ACKER, Louis K., JR., Min. Engr 565 Highland Place, Bellevue, Pa. '08

Jan 1, 1917

By Jacques B. Wertz

Among the parameters to be considered in the continuous search for new base-metal deposits, there often is a stratigraphic controlling factor that seems instrumental in the localization of ore. In British Columbia, for instance, the Upper Triassic as well as Lower Jurassic volcanics mixed with sediments are a useful indication in the search for copper while, in some parts of Australia, rhyolite bodies seem to be the favorable indicator, and this always within the geosynclinal environment. In Arizona, this stratigraphic factor becomes highly significant and it will be shown here that a large number of ore deposits are to be located around the flanks of ancient calcareous basins or depressions, preferentially corresponding to a certain optimum thickness as revealed by isopachs. The Martin limestone, of Devonian age, is already known for its basal O'Carroll bed which coincides with mineralization at places, and this is a relatively minor control. However, several limestone basins outlined by isopachs are in reality of greater importance as they localize mining districts. Indeed, most mines are found to coincide with a specific thickness of limestone while occurring simultaneously close to major, regional fracture intersections. The regional fractures in question were interpolated and extrapolated from known, important fault expressions, integrating quite well with the existing geology and further confirmed by minor criteria such as contacts, igneous plugs, axes of elongation of batholiths, dikes, etc. Although elements of subjectivity remain, this grid of fractures can be used quite successfully as a working hypothesis in the search for ore. Results of the present study which superposes major structural

Jan 1, 1971

By J. R. Bridge, D. A. Vaughan

The phase diagram of the Zr-H system over the range 0 to 65 atomic pet was determined by high temperature X-ray diffraction methods. Results show a eutectoid between a zirconium and the hydride phase. The eutectoid temperature was established at 560±10°C with a eutectoid composition of 42*3 atomic pet H. The hydride phase of the lowest hydrogen content is stable only above the eutectoid temperature, but is formed and retained in a metastable state during reaction of zirconium with hydrogen at temperatures below 560°C. One hydride phase is indicated that exists over the composition range 55 to 65 atomic pet H. RECENT increase in the industrial importance of zirconium has stimulated several investigations of the reaction of zirconium with hydrogen. Review of the literature on interpretation of absorption isotherms' ' shows that attempts were made to relate the observations to the room temperature hydride phases reported by Hagg.3 However, more recently Schwartz and Mallett' reported the existence of a new hydride phase, isomorphous with the lower hydride in the Hf-H system described by Sidhu.4 This phase was found adjacent to the metal in a diffusion gradient sample. In addition to the new phase, Schwartz and Mallett reported on only two of the five hydrides found by Hagg. Gulbransen" confirmed the existence of only three hydrides of

Jan 1, 1957

By George Stern

THE purpose of this investigation has been to study one method for making ordinary carbon steel by the powder metallurgy technique. This method con- [ ] sists of pressing and subsequently sintering an intimate mixture of iron powder and graphite in a suitable atmosphere to produce a steel. Two types of iron powder have been studied, electrolytic and reduced. The sintering of mixtures of loose carbonyl iron and carbon black for several hours at 1000° to 1100°C. (1830° to 2010°F.), followed by forging of the resultant ingots to bars, has been studied by Offermann.1 Trail' has reported on the properties of hydrogen-reduced and electrolytic iron powders, both containing 0.5 per cent carbon. Methods for making steel bodies by powder metallurgy have also been sug- [ ] gested by Goetzel,3 who recommends the addition of steel powder of well-defined carbon content to pure iron powder, and Volterra,4 who suggests compaction and subsequent sintering of a mixture of steel powder, iron oxide and iron powder. Additional methods for making steel bodies by powder metallurgy have been reported in the literature by Koehring,5 Allen,6 Balke,7 Wulff,8 Boegehold,9 and others. 10,11,12 It is felt that the method of pressing iron powder and graphite, as described herein, lends itself best to production because of the lubricating action of the

Jan 1, 1946

By D. A. Vaughan

COMPOUNDS in the U-N system have received little attention since the work of Rundle, Baen-ziger, Wilson, and McDonald in 1948.' They described the three nitrides UN2, U2,N2, and UN as the only phases in this system. The region between UN and U,N, was reported to consist of the two phases while the region between U,N, and UN, is a homogeneous solid solution in which the U,N3, structure transforms with increasing nitrogen content into the UN, structure. This report presents the results of an X-ray diffraction study of the phases present in the region of the diffusion gradient on uranium reacted with nitrogen at several temperatures between 500" and 915°C. Several samples of uranium used in U-N gas-metal reactions by Mallett and Gerds were available for X-ray diffraction study of phase composition through the diffusion gradient. X-ray diffraction data were obtained using filtered iron radiation at intervals through the diffusion layer of the several samples on filings or turnings at approximately 0.001 in. increments down to the base metal. Representative X-ray diffraction patterns from various layers through the case on uranium after nitriding at 850°C are shown in Fig. 1. These data show that three different phases are present in the

Jan 1, 1957

By T. H. Courtney, G. W. Pearsall, J. Wulff

The mechanism, of the decrease in transition temperature of Nb3Sn was studied. Presintered Nb3Sn powder compacts were heated in a dynamic vacuum at elevated temperatures. Loss of tin resulted from these heat treatments and transition temperature as a function of tin loss was discontinuous at a critical value of tin loss. In general, decreases in transition temperature were correlated with deviations from AS a class, the A15 structure-type (also known as Cr3O or ß W) compounds have the highest superconducting transition temperatures.' In this class are stoichiometry and presence of vacancies in niobium sites. The effect of vacancy distribution on the physical properties of Nh3Sn is considered. It is concluded that the close-packed atomic A chain in the A3B A15 structure must be preserved both in coutinuity and direction if good superconducting properties are to he obtained. tempting to associate these high transition temperatures with the most unique crystallographic feature of the A3B structure: the three close-packed, orthogonal chains of A atoms.'0"' There are at least three principal mechanisms by which the perfection of these "A-atom chains" could be interrupted: changing stoichiometry, inducing disorder, or introducing vacancies. Departures from stoichiometry in either direction in V3Ga lower the transition temperature.7'8 In niobium-

Jan 1, 1965

By Carle Hayward

THE effect of copper on steel has been studied by numerous investigators. Before modern testing methods had been developed, blacksmiths noted red shortness in iron, the cause for which was ascribed to the presence of copper. Numerous papers have been published on the corrosion of steels containing various amounts of copper, and a few writers have discussed the effect of copper on the mechanical properties of steel. The purpose of the investigation described in the following paper was to obtain additional data on the mechanical properties of medium-carbon steel containing small quantities of copper. Among those who have published results of mechanical tests on copper steels are Ball,1 who states that copper increases the tensile strength and 'hardness but lowers the elongation. Stead2 states that copper steels closely resemble nickel steels containing equivalent percentages of nickel,, as regards tensile strength, resistance to shock, corrosion and hardness. Wigham 5 found that copper in small amounts had no injurious effect on steel. Breuil4 found that with 1 per cent. carbon, copper lessened the brittleness of steel and in low-carbon steel it increased the tensile strength and lowered the ductility slightly. H. H. Campbell 5 states that copper up to 0.25 per cent. slightly raises the elastic limit, elongation and reduction of area.

Jan 1, 1918

By F. L. Holderreed

A choosy in what they would smelt. The furnace charge had to be coarse, and it had to be rich. They discarded fines in excess of about 1/10 the total weight. They wanted 10% copper content and fussed about anything with as low as 5%. They concentrated the copper content of the charge as much as they could by prior selection. They roasted off enough sulfur to further enrich the copper content of the succeeding fall of matte (a melt of cuprous and ferrous sulfides or Cu2S.FeS). Then they desulfurized the iron and fluxed it by carefully adding silica (quartz, not silicates) for a slag of lower density than the cuprous sulfide (Cu2S or white metal). After skimming off the slag, they further desulfurized the white metal by blowing the molten bath with compressed air. The result was blister copper. Yesterday Their techniques and furnaces? Some experimented with mechanically rabbled roasters, but their standard roasting practice was burning coarse sulfide ore in 250-ton heaps. These heaps, approximately 24 x 24 x 6 ft, were burned for about 75 days down to 6-10% sulfur. The turnaround time for a given roasting position was 100 days. Assuming the base was a hearth, the calculated rate of treatment was on the order of 0.004 tpd per sq ft.

Jan 1, 1971

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

THE tensile and notch tensile ductile-to-brittle transition characteristics of several refractory metals and alloys have been well documented.1-3 Electron-beam melted tantalum and columbium have been shown to retain excellent ductility at very low temperatures. Some indications of brittle behavior (low ductility and cleavage fracture) were observed with columbium tested at -253oC, but no similar effects were noticed with tantalum. Increasing the interstitial oxygen content in these two materials resulted in the detection of indications of brittle behavior at higher temperatures, although good ductility was retained in both bases at -196°C when they contained about 1 at. pet 0. Detailed descriptions of the impact transition behavior of these two materials at various purity levels have not been available. This technical note describes the effect of interstitial oxygen on the impact properties of wrought, fibered tantalum and columbium and compares the transition behavior to the previously determined tensile transition characteristics. Tantalum and columbium impact specimens with three different interstitial oxygen levels indicated in Table I were tested at temperatures ranging from -196o to 300°C. Oxygen additions were made to 1/2-in.-diam bars of electron-beam melted material in a Seiverts Apparatus. The oxygenated bars were then homogenization-annealed to obtain uniform cross-section hardnesses and swaged to

Jan 1, 1964

By B. Kopelman, C. C. Gregg

THE reduction of tungstic oxide to tungsten metal powder by hydrogen is a process by which one might expect the resultant metal powder to he porous. In- deed, sponge iron, prepared by rcduction of the oxide in a reducing gas, is generally accepted as quite porous. with pores large enough to be seen readily under the optical microscope at relatively low magnifications. However, any pores that may exist in tungsten metal powder are not resolved by the optical microscope, and apparently, not even by the electron microscope. Fig r shows commercial tungsten powder magni- fied at I0,000 X by the electron microscope,' both etched and unetched. In an earlier paper by one of the authors,* the existence of ports in tungsten powder was required to explain adequately the particle size changes occurring during the reduction of tungstic oxide. The inability to detect these pores under the electron microscope at 10,000 X implies that these {pores} are of a size of 100 A units or less. (This in itself is by no means proof that pores above 100 A would not exist, since polishing effects on the specimen might smear up holes of such small magnitude). If, then, these pores are less than IOO A. and of the order of molecular size, then the density of the metal powder should be

Jan 1, 1949

By B. Fagerberg, P. H. Fahlstrom

Crushing and grinding practice in Sweden follows closely the international pattern. Certain special circumstances, however, have had an influence on its development. Most mines are worked underground. These mines are either quite small or very large. Sulfide ores are commonly treated by custom milling and, apart from the cement industry, the rock species treated are hard and abrasive. Another important factor is the increasingly strict requirements placed on the mechanical condition of different products, especially lump ores and coarse iron-ore concentrates. Increasing requirements are being placed on the concentrate grade to suit the new steel processes. As a result, iron ore beneficiation has expanded considerably for the production of fine pelletizing concentrates. This applies especially to magnetite ores in the intermediate phosphorus range 0.1-1% P. In 1969, about 5.5 million tons of pellets will be manufactured. It should be pointed out, however, that fairly large quantities of coarse products are still being made at mills where the right conditions are available. Crushing and grinding is also of great importance in the production of rich concentrates at high recovery from sulfide ores. In fact, a large part of the development work on the concentration of sulfide ores has been devoted to the crushing and grinding processes. Boliden has played an important role in this connection.

Jan 10, 1969

By M. J. Salkind

In discussing the possible contribution of plastic deformation to neck growth during sintering, Wilson and Shewmon State that Lenel, Ansell, Salkind, and Early34, 35 concluded that dislocation flow is the rate-controlling process in sintering under zero external load. The experiments cited34, 35 were done with applied external loads, and the conclusions were that the same kinetics could be controlling sintering due to the force of gravity with no additional applied load. The effect of gravity on sintering behavior was previously cited.34, 31 In addition, Wilson and Shewmon argue that the conclusions of Refs. 34 and 35 are doubtful because the strain rate is proportional to stress for plastic flow. This assumption is true only for certain kinds of plastic flow such as Nabarro-Herring Microcree38 As Early, Lenel, and Ansell point out3' plastic flow, based upon dislocation movement, can exhibit strain rates which exhibit a power law relationship to the applied stress.39, 40 Wilson and Shewmon also doubt the results of Refs. 34 and 35 because the stresses in the necks are too small for x/a > 0.1. This is true, and the experiments described in Refs. 34 and 35 were done for small values of %/a. The conclusion was that plastic flow by dislocation movement was important during the early stages of sintering when x/a is small.

Jan 1, 1968

By R. Ward Grosz

Reasonable and timely solutions to the complicated mathematical calculations involved in the mine planning, economic evaluation and slope stability studies related to the Ruth Mine would not have been feasible without the modern digital computers. The Ruth Mine was a prosperous underground copper operation in east central Nevada from 1915 to 1948, when rising mining costs finally exceeded the value of the ore. A substantial reserve of porphyry copper remained in the ground, but until recently all economic evaluations indicated that it was at best a marginal operation and a relatively poor risk of capital. There has been a steady progress in improving all aspects of surface mining since the first steam shovel started stripping overburden; however, developments in just two rather specialized areas proved to be critical in changing the Ruth Mine from a reserve of mineralized rock to an economically attractive orebody. One involved the progress made in recent years in the science of slope stability. Applying the latest techniques in this field to mine planning resulted in reducing the stripping ratio from 6.0:l to 4. 2:l. The other major factor was the efficiency and cost performance of large capacity haulage trucks which made it feasible to go down over 1100 ft. in an open pit and recover ore with a high stripping ratio economically.

Jan 1, 1969

By J. S. Kirkaldy, R. J. Brigham

AS part of a program to investigate the diffusive properties of dilute ternary austenites we have made a determination of the effect of chromium on the activity of carbon in ? iron. Samples of pure iron and Fe-Cr alloys were simultaneously equilibrated at 1000°C with atmospheres of controlled CO/CO2 ratio following the procedures of Darken and Gurry 1 and smith.' The 0.020 in. thick samples were analysed for carbon by microcombustion analyses3 to yield a set of isoacti-vity curves. The latter were converted to activity coefficient (standard state at infinite dilution) plots by combination with Smith's data2 for the activity of carbon in pure iron. Table I shows the compositions of the base alloys used while Fig. 1 shows the experimental results superimposed on a set of curves generated by the relation In?C=6.9NC- 10.7 Ne In the notation of wagner4 the interaction parameter is the second coefficient on the right, Sgr = - 10.7 This can be compared with a rather inaccurate value deduced from the transient equilibrium diffusion data of Kirkaldy et al.' as The authors are indebted to the American Iron and Steel Institute for financial support. This material is condensed from a B.Sc. Thesis submitted to Mc-Master University by R.J.B.

Jan 1, 1963

By P. K. Koh, H. A. Lewis, H. F. Graff

New data on the distribution of silicon between slag and carbon-saturated iron at 1600Oand 1700OC are presented which, in combination with previously published data, permit the determination of silica activities over a broad range of compositions in the CaO-Al2O3-SiO2 system. The distribution of silicon between graphite-saturated Fe-Si-C alloys and blast furnace-type slags in equilibrium with CO has been described in previous publications.1"3 In this past work the silica-silicon relation was established at temperatures of 1425" to 1'700°C for slags containing up to 20 pct A12O3. This paper presents the results of additional studies at 1600" and 1700° C which extend the silicon distribution data at these temperatures for CaO-A12O3-SiO, slags over a range from zero pct Al2O3 to saturation with Al2O3, or CaO.2Al2O3. The upper limit of SiO2 is set by the occurrence of Sic as a stable phase when the metal contains 23.0 or 23.7 pct Si at 1600" or 1700°C, respectively. The activity of silica over the expanded range is determined directly from the distribution data.3 Recently4-7 other investigators have studied the activities of SiO, and CaO, principally in the binary system, using different methods and obtaining somewhat different results. EXPERIMENTAL STUDY The experimental apparatus and procedure have been fully described in previous publications.1, 3 Six new series of experimental heats have been made, four at 1600° and two at 1700°C. Master slags of several fixed CaO/Al203 ratios were pre-melted in graphite crucibles, and these were used with additions of silica to prepare the initial slag for each experiment. Slag and metal were stirred at 100 rpm and CO was passed through the furnace at 150 cc per min. The initial sample was taken 1 hr after addition of slag at 1600°C or 1/2 hr after addition at 1700°C. The run was normally continued for 8 hr at 1600°C or 7 hr at 1700°C, and the final sample was taken at the end of this period. Changes in Si and SiO2 content indicate the direction of approach to equilibrium, and in a series of runs where the approach is from both sides this permits approximate location of the equilibrium line. Fig. 1 shows the results of such a series of 15 runs at 1600°C for slags of CaO/Al,O3 = 1.50 by weight. Figs. 2 and 3 record other series at 1600°C and Fig. 5 a series at 1700°C with fixed CaO/Al0 ratios. The results of the experiments at 162003°C have been reported in part in a preliminary note.3 In the experiments recorded in Figs. 4 and 6, the slags were saturated with A12O3 (or with CaO.2A12O3 within its field of stability) by suspending a pure alumina tube in the melt during the course of the run. The final slag analyses were used to establish the liquidus boundaries8 in the stability fields of CaO.2Al2O3 and of Al20,. ACTIVITY OF SILICA The free-energy change in the reaction has been calculated by Fulton and chipman2 from recent and trustworthy data including heats of formation, entropies, and heat capacities. The more recent determination by Olette of the high-temperature enthalpy of liquid silicon is in satisfactory agreement with the values used and therefore requires no revision of the result which is expressed in the equation: SiO2 (crist) + 2C (graph) = Si + 2CO(g.) [1] &F° = + 161,500 - 87.4T The standard state for silica is taken as pure cristobalite and that of Si as the pure liquid metal. Since the melts were made under 1 atm of CO and were graphite-saturated, the equilibrium constant for Eq. [I] reduces to K1 = asi /asio2. The value of this constant is 1.77 at 1600°C and 16.2 at 1700°C. Through K1, the activity of silica in the slag is directly related to the activity of silicon in the equilibrium metal.

Jan 1, 1960

By E. A. Steigerwald, G. L. Hanna

The influence of work-hardening exponent on the variation of fracture toughness with material thickness was studied for high-strength steel, aluminum, and titanium alloys. The results indicate that, when materials are compared at similar fracture toughness to yield strength ratios, the material with the lower work-hardening exponent undergoes the transition from flat to slant fracture at a larger thickness than material with a high work-hardening exponent. In the thickness range where complete slant fracture is obtained the reverse is true and a lower work-hardening exponent results in a lower fracture toughness. The influence of work-hardening exponent on fracture toughness is, therefore, dependent on the particular fracture mode. In the transition region a low work-hardening exponent is beneficial for fracture toughness while in the 100 pct slant region it is detrimental. THROUGH the use of fracture mechanics analyses, the influence of geometric variables on the crack propagation resistance of structures can be interpreted with reasonable consistency. However, in order to gain a more complete understanding of the fracture process, the influence of material parameters on crack propagation must be defined and coupled to the macroscopic fracture mechanics approach. The work-hardening exponent, which characterizes specific material behavior, may serve as an effective parameter to allow some degree of coupling to be accomplished. In the extension of a crack in a specimen of suitable dimensions the propagation process occurs in a stable manner when the crack extension force is balanced by the resistance to crack extension, which exists in the material at the crack tip. As the applied stress, and therefore the crack extension force, on the specimen increases, the resistance also increases primarily because the effective plastic zone at the crack tip, which is the main energy absorption process, becomes larger. Since the work-hardening rate of a material influences the stress-strain relationship, it will also influence the energy absorption process in the plastic enclave at the crack tip and hence should have an effect on crack propagation. A number of studies have been made correlating the strain-hardening exponent or the strain to tensile instability with the ability of a material to resist fracture. Gensamer1 concluded that a low-strain-hardening exponent would result in a steep strain gradient at the base of a notch. He reasoned that a large work-hardening coefficient would result in high-energy ab- sorption due to the increased area under the stress-strain curve. Larson and Nunes2 experimentally observed in Charpy tests on steels heat-treated to below 200,000 psi yield strength that the energy to failure in the fibrous mode, i.e., above the brittle-to-ductile transition temperature, was logarithmically related to the strain-hardening exponent. In order to avoid the complicating effects present in studying materials which undergo a brittle-to-ductile transition, Ripling evaluated the notch sensitivity of a variety of fcc metals with varying work-hardening exponents.3 The results indicated that the relative notch sensitivity, as determined from tests on specimens with a sharp notch, decreased with increasing values of strain hardening. Although the energy required for ductile or fibrous fracture increases with increasing work hardening, high-strength steels often exhibit improved crack propagation resistance when heat-treated to obtain low values of strain hardening.4,5 An analysis of whether low strain hardening is beneficial or detrimental to crack propagation resistance must depend on the particular fracture criterion involved. At temperatures where the material is relatively ductile and the development of a critical strain is required for fracture, high strain hardening increases the energy required to produce failure. In the transition region and below, however, a critical stress law appears to be valid6 and a low rate of work hardening may produce superior resistance to semibrittle crack propagation. The experimental program is aimed at studying these possibilities and determining the specific influence of strain hardening on the crack propagation resistance of several high-strength materials. MATERIALS AND PROCEDURE The alloys, chosen as representative of various classes of high-strength materials, are summarized in Table I. The heat treatments evaluated along with the smooth tensile properties are presented in Table 11. Pin-loaded sheet tensile specimens were employed to determine the smooth tensile properties. A strain gage extensometer (measuring range 0.200 in.) was used at a strain rate of 0.02 in. per in. per min. The work-hardening exponents were determined from the stress-strain curves generated in the smooth tensile tests and the assumption that the portion of the stress-strain curve beyond the yield point can be described by the power relationship: where a is the true stress, P is the true plastic strain,

Jan 1, 1969

By A. Szirmae, Hsun Hu

The early stages of recrystallization in a 70 pct cold-rolled Si-Fe crystal of the (110) (0011) orientation were studied with a Siemens electron microscope. Orientation studies based on electron-diffractzotz. patterns confirm the results of previous texture analysis. The driving energy for recrystallizatior and the critical radius for growth were calculated from the dislocation energy and the energy of the subgrain bourzdaries, and it was found consistent with the observed size of the recrystallized grains. The recrystallization characteristics of crystals with different initial orientations are discussed. The recrystallization of cold-rolled (110)[001] crystals of Si-Fe has been widely studied by various investigators.1-4 Their results on both deformation and annealing textures are in good agreement. The rolling texture after 70 pct reduction consists mainly of two crystallographically equivalent (111) [112] type textures and a minor component of the (100) [011] type. The latter is derived from the deformation twins, or Neumann bands, which are formed during the early stages of deformation and later rotate to the (100) [011] orientation upon further rolling reduction. Between the two main (111) [112] type textures, there is some orientation spread, because of which very low intensity areas appear in the pole figure. If these very low intensity areas are considered to be a very weak component in the texture, then a (110) [ 001 ] orientation may be assigned to them. When this rolled crystal is annealed at a sufficiently high temperature for recrystallization, the texture returns to a simple (110) [001]. The purpose of the present investigation was primarily to seek a better understanding of the recrystallization process by using the electron transmission technique. The (110) [0011 type of crystal was selected because orientation data for it are well known from previous studies with conventional techniques. Direct observations on the recrystallization of such a crystal have also been made by using a hot-stage inside the electron microscope, and the results will be reported in another paper. MATERIAL AND METHOD A single-crystal strip of the (110) [001] orientation was prepared from a commercial grade 3 pct Si-Fe alloy by the strain-anneal technique.= The strip was approximately 0.014 in. thick, and was rolled 70 pct at room temperature to a thickness of 0.004 in. Specimens were cut from the rolled strip and were annealed in a purified hydrogen or argon atmosphere. They were then electrolytically polished in a chromic-acetic acid solution to very thin foils. Best results were found by polishing first between two narrowly spaced flat cathodes with the specimen edges coated with acid-resisting paint, followed by polishing between two pointed electrodes until a hole appeared in the center as described by Bollmann.6 It was found that a thin transparent film always formed along the thin edges of the polished specimen. This film was then removed by rinsing the specimen very briefly in a solution of alcohol with a few drops of HF or HCl. RESULTS AND DISCUSSION 1) The Deformed Crystal. From the electron-diffraction patterns taken at various areas of an as-rolled specimen, the texture components as deduced - from ordinary pole-figure analysis were confirmed. Over most of the areas where orientation was examined, a (111) pattern with a [112] direction parallel to the rolling direction was obtained. This corresponds to the main deformation texture of the (111) [112] type. In a few areas the diffraction pattern was (100) [Oil], corresponding to the minor-texture component derived from the Neumann bands. The (110) [001] orientation, which corresponds to the very weak intensity area in the pole figure, was found infrequently. A typical example of the deformed matrix having the (111) type main texture is shown in Fig. 1, where (a) is the microstructure and (b) is the diffraction pattern taken from that area. It was also frequently observed that in other areas more or less continuous rings of weaker intensity were superimposed on the simple (111) diffraction pattern, suggesting the presence of a wide range of additional orientations. Other evidence indicated that the recrystallization characteristics are different in these two different types of areas. The hot-stage observations which provide this evidence will be discussed in another paper. AS shown in Fig. l(a), numerous dislocation-free areas of very small size are embedded in the "clouds" of high-dislocation density. This indicates that the deformation of a single crystal, even after a rolling reduction of 70 pct, is far from uniform on a micro-

Jan 1, 1962

By D. W. Rudd, D. W. Vose, S. Johnson

The permeability of Mo-0.5 pel Ti to hydrogen was investigated over a limited range of temperature and pressuire (709° to 1100°C, 1.i and 2.0 atm). The resulting permeability, p, is found to obey the The experimental data justifies the permeation mechanism as a diffusion contl-olled pnssage of Ilvdrogen atoms through the metal barrier. 1 HE permeability of metals to hydrogen has been investigated by a number of workers and their published results have been tabulated by Barrer' up to 1951. Since most of the work on the permeability has been accomplished prior to this date, the compilation is fairly complete. Mathematical discussion of the permeability process has been reported by Barrer, smithells, and more recently by zener. From these efforts several facts are observed. First, the permeability of metals to diatomic gases involves the passage through the metal of individual atoms of the permeating gas. This is evidenced by the fact that the rate of permeation is directly proportional to the square root of the gas pressure. Second, the gas permeates the lattice of the metal and not along grain boundaries. It was shown by Smithells and Ransley that the rate of permeation through single-crystal iron was the same after the iron had been recrystallized into several smaller crystals. Third, it has been observed that the rate of permeation is inversely proportional to the thickness of the metal membrane. Johnson and Larose5 verified these phenomena by measurirlg the permeation of oxygen through silver foils of various thicknesses. Similar findings were noted by Lombard6 for the system H-Ni and by Lewkonja and Baukloh7 for H-Fe. Finally, it has been determined that for a gas to permeate a metal, activated adsorption of the gas on the metal must take place. Rare gases are not adsorbed by metals, and attempts to measure permeabilities of these gases have proved futile. ~~der' found negative results on the permeability of iron to argon. Also, Baukloh and Kayser found nickel impervious to helium, neon, argon, and krypton. From what was stated above concerning the dependence of the rate on the reciprocal thickness of the metal barrier, it is seen that although adsorption is a very important process, at least in determining whether permeation will or will not ensue, it is not the rate determining process for the common metals. A case in which adsorption is of sufficient inlportance to cause abnormal behavior has been noted in the case of Inconel-hydrogen and various stainless steels.'' APPARATUS The apparatus used in this study is shown in Fig. 1. The membrane is a thin disc (A), but is an integral part of an entire membrane assembly. The entire unit is one piece, being machined from a solid ingot of metal stock. When finished, the membrane assembly is about 5 in. long. Two membrane assemblies were made; the dimensions of the membranes are given in Table I. The wall thickness is large compared to the thickness of the membrane, being on the average in the ratio of 13 to 1. There exists in this design the possibility that some gas may diffuse around the corner section of the membrane where it joins the walls of the membrane assembly, If such an effect is present, it is of a small order of magnitude, as evidenced by the agreement of the values of permeability between the two membranes under the same temperature and pressure. A thermocouple well (B) is drilled to the vicinity of the membrane. The entire membrane assembly is then encased in an Inconel jacket and mounted in a resistance furnace. The interior of the jacket is connected to an auxiliary vacuum pump and is always kept evacuated so that the membrane assembly will suffer no oxidation at the temperatures at which measurements are taken. The advantages of this configuration are: 1) there are no welds about the membrane itself, so that the chance of welding material diffusing into the membrane at elevated temperatures is remote. 2) It is possible to maintain the membrane at a constant temperature. Since the resulting permeation rate is very dependent upon temperature, it is advisable to be as free as possible from all temperature gradients. 3) It is possible to obtain reproducible results using different specimens. The only disadvantage to this configuration is the welds (at C) in the hot zone. The welding of molybdenum to the degree of per-

Jan 1, 1962

By I. R. Kramer, L. J. Demer

T. H. Alden and R. L. Fleischer (General Electric Research Laboratory)— The authors' results indicate clearly and, we believe, significantly that during tensile deformation the surface layers of an aluminum crystal are hardened more severely than the interior of the crystal. A probable explanation of this effect, as the authors indicate, is that dislocations in the primary slip system may be obstructed at the surface or, it should be added, near the surface. The intent of this discussion is to show that the oxide film on aluminum is not likely to be responsible for this effect, but that the results can be understood if it is assumed the secondary slip is more active in the surface layers than in the interior. Prior study has shown that the principal mechanical effect of an oxide film on a single crystal is to raise the yield stress while leaving the rate of strain hardening during the initial deformation relatively unaffected.33 Since the yield stress is unchanged during polishing in the present case, we conclude that continual removal of the oxide film exerts a small effect on the plastic hardening.* It appears that the hardening interactions are occurring not only at the immediate surface, but to an appreciable depth below it, although with decreasing severity. For example, Kramer and Demer found that with removal of 0.004 in. from a specimen, the easy glide region was extended somewhat; but the yield stress did not decrease. The initial yield stress was recovered only after 0.041 in. was removed. Since a very brief polish would permit dislocations trapped behind a surface film to run out,34 extra dislocations must, instead, be trapped to a considerable depth below the surface. The same conclusion is drawn from the observation of decreasing hardening slope with increasing surface removal rates. If the hardening interactions were only at the immediate surface, a full softening effect would be observed at some small removal rate. The view is taken here that strain hardening is principally caused by small amounts of secondary slip.35 The secondary dislocations will interact in various ways with the primaries, interfering with their motion and causing them to accumulate in the crystal. Prior studies of easy glide have shown Diehl's model of hardening to be qualitatively consistent with the effects of impurities,36 of temperature,36 and of crystal size.37 On this basis the enhanced hardening of the surface layers in aluminum arises from increased secondary slip at and to some depth below the surface. Selective removal of this hardened layer is expected to decrease the measurable "bulk" hardening, the effect increasing with the removal rate and decreasing with the applied strain rate. We suggest that the stress on secondary systems is raised by the bending moments arising from interactions with the grips during the deformation. This stress from the grips has been shown to be a maximum37 near the surface, and hence, increased secondary slip should result. Prior investigations of grip effect:; indicate that as the grip stresses are raised by changing the crystal shape, the easy glide slope increases while the extent of easy glide decreases.38-40 It has been shown also that bending moments superimposed during tensile testing may either decrease easy glide, when supporting the moments caused by gripping, or increase it, when cancelling the gripping moments.38 This interpretation of the authors' results, emphasizing the special importance of secondary slip near the surface, is also consistent with the earlier results of Rosi.41 Copper crystals alloyed with silver in the surface layer show greatly increased easy glide compared with pure copper. In addition, the easy glide slope is reduced. The effect of bulk alloying in extending easy glide has been well established and has been interpreted as indicating the relative difficulty of secondary slip in alloy crystals. Since non-basal glide is difficult in zinc crystals, the effects of surface removal during deformation may be less important. Experiments to test this idea are in progress. I. R. Kramer and L. J. Demer (authors' reply)—The authors wish to thank Dr. Alden and Dr. Fleischer for their discussion. Our interpretation of the data in the paper is that dislocation motion is obstructed by "debris" which starts to form at the surface and extends towards the interior of the crystal with further plastic deformation. The fact that we did not find a reversion from Stage II to Stage I by surface removal shows that in Stage II the "debris" fills the entire cross-section of the specimen. Drs. Alden and Fleischer take the view that bending stresses due to the grips are responsible for the

Jan 1, 1962