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By R. M. N. Pelloux

This study of aluminum-copper alloys had two aims: 1) To determine the effect of the amount and distribution of a second phase, CuAl2, on the creep-rupture strength, ductility, and fracture characteristics of the alloys. The work of Gemmell and grant' on single-phase aluminum-copper alloys provided a basis for the present study. 2) To attempt to provide a relation between the microstructure and strength of two-phase alloys deformed at comparatively high temperatures (greater than 0.45 T,). The creep behavior of the two-phase magnesium alloys Mg;Ce and Mg-A1, has been treated by Roberts. 9 In work reported by Sully and Hardy4 and by Underwood, Marsh, and Manning~ on A1-Cu two-phase alloys, and also in a portion of the work of Gemmell and grant,' aging took place during the creep tests. 'In the present work, overaged aluminum-copper alloys were subjected to creep deformation at two temperatures, 500 and 700OF. The overaging treatments to produce the precipitate dispersions were performed prior to the test, at temperatures which were the same as the ultimate respective test temperatures. Hence, the present study is concerned with the creep behavior of stable (in contrast to "underaged") two-phase A1-Cu alloys, i.e., alloys in which no depletion of the solid-solution matrix occurred during: creep. MATERIALS AND PROCEDURE A 2 and a 3 pct Cu alloy, supplied by Alcoa, were studied; Table I shows the compositions. The grain size of the specimens, 0.9 to 1.0 mm, was achieved by annealing the machined test bars for 2 hr at 1000°F, followed by furnace-cooling to 900°F, and homogenizing for 4 hr. Both compositions are in the single-phase condition at 900°F. Two types of overaged dispersions, termed "over-aged I" and "overaged 11" were prepared after the grain size and the homogenization anneals. The overaged I alloys were prepared by quenching to room temperature after homogenization, aging at either 500' or 700°F for 72 hr, and air-cooling to room temperature. The overaged I1 alloys were prepared by furnace-cooling after homogenization, to either 500' or 700°F, and holding at the necessary temperature for 72 hr. The times for furnace-cooling from 900°F to 700° and 500°F were, respectively, about 2 and 3.5 hr. The structures of the A1-2 pct Cu alloys are shown in Fig. 1 (overaged I) and in Fig. 2 (overaged 11). A comparison of Figs. 1 and 2 shows that in the overaged I alloys the precipitate particles along the grain boundaries are much more closely spaced and the grain boundaries are straighter than they are in the overaged I1 alloys. Further, the particle size and spacing in the grains are smaller than in the overaged I1 alloys. Microstructures of the A1-3 pct Cu alloys have not been shown; the structures of these alloys differed from those of the A1-2 pct Cu alloys only in that the distribution density of the particles was greater. The creep specimens had a gage section 1 in. long with a diameter of 0.155 to 0.195 in. Before testing, specimens were electropolished in a solution of 100 cc glacial acetic acid, and 30 cc of 60 pct perchloric acid, at 40' to 50°F, at 24 v. The specimens were kept refrigerated prior to testing to avoid precipitation at room temperature. Constant stress creep tests were conducted; the load was applied 75 min after heating of the specimens to test temperature had begun. EXPERIMENTAL RESULTS Creep-Rupture—Fig. 3 shows the log stress-log rupture life plotfor the overaged alloys studied, and also for the underaged A1-2 pct Cu alloy.' At 700°F, the stress-rupture life relationship is nearly independent of both the amount of precipitate (i.e., composition) and of the type of overaging treatment (i.e., precipitate dispersion). At 500°F it is apparent that the increase in rupture life that was ex-

Jan 1, 1960

By A. Lubinski, J. L. Logan, W. S. Althouse

A4ost gas twells and flowing oil wells are completed and treated through a string of tubing and a packer. Changes in temperature and in pressure inside or outside the tubing will: (I) if free motion of the tubing inside the packer is permitted, increase or decrease the length of the rubing; or (2) if free motion is prevented, induce forces in the tubing and on the packer. If pressure inside the tubing is greater than outside, the tubing may buckle helically even in the presence of a packer-to-tubing tension. The tubing will always buckle, and much more severely, if free motion is permitted. The buckling may be prevented by pulling the tubing in sufficient tension. The prediction of these forces and tubing movement has here to fore been based upon calculations that did not inciude helical buckling. This paper preseitts means with which these length or force changes can be calculated while taking into account the effect of helical buckling. To avoid damaging formations, failure of remedial operations, or damage to the tubing or packer, application is made to practical problems involving calculations of the required length of seals, amount of sluckoff or tension, and prevention of permanent corkscrewing. INTRODUCTION Leakage of a packer may result in costly failures of such operations as squeeze cementing, hydraulic fracturing, etc. To avoid such failures, the authors are often asked questions pertaining to the length of necessary seals, the amount of necessary slackoff, etc. Published work' does not take into account helical buckling of tubing. Investigation of helical buckling was prompted by the fact that allowance must be made for this phenomenon in order to provide relevant answers. In the past, theoretical work on helical buckling was confined to conditions for which such buckling does not The mathematical treatment of behavior in a buckled condition, given in the Appendix, is novel. Assumptions upon which this investigation is based are listed and discussed in a special section. The following are a few of the many kinds of problems which may be solved with this paper. 1. Consider a packer in which tubing may move. Such movement will occur after pressures and temperature are changed. The paper provides means for: (a) calculating the amount of such movement and, therefore. the required length of seals; and (b) calculating the necessary amount of initial slackoff, for which there is no danger of unsealing the packer, if the length of seals is given. Such calculations, as well as those which follow, tully take into account the fact that part of the movement ib due to elastic helical buckling of the lower part of the string. This buckling may occur even in tubing under tension. Insufficient initial slackoff for a given length of seals, or insufficient length of seals for a given slackoff, may result in costly failures. A field case of such a failure will be given further in this paper. 2. In the case in which tubing cannot move in the packer, changes of pressure and temperature result in tubing-to-packer forces and forces in the tubing above the packer, both of which may be calculated. This knowledge is important because, if these forces are too large, the) could damage the packer or the tubing. 3. For wells in which wireline tools are to be run through the tubing, the paper provides means to keep the tubing from buckling, thereby permitting free passage of tools. 4. In deep wells, mainly in the presence of large casing, tubing may become "corkscrewed", i.e., take a permanent helical set. A field case is described further in the text. Using this paper, one may calculate in advance conditions under which permanent corkscrewing would occur, and then take preventive steps. HELICAL BUCKLING Consider a string of tubing, freely suspended in the absence of any fluid inside casing, as shown in Fig. I(a). Now consider an upward force F applied at the lower end of this tubing. This force compresses the string; and if the compression is large enough (which is always the case in actual problems), the lower portion of the string will buckle into a helix, as shown in Fig. 1 (b). The lower end of the tubing is subjected to a compression F. This compression decreases with the distance from the bottom and becomes nil (neither compression nor ten-

By Earl G. Alexander, W. R. Runyan

The nature of silicon growths which form on amorphous silicon dioxide during epitaxial deposition in unmasked areas was investigated. Octahedral silicon crystals nucleate and grow on the oxide at pinholes, adjacent to foreign matter, and probably at oxygen-deficient sites. Generation of these oxygen-deficient sites on the oxide surface is shown to be thermody-namically favorable under usual deposition conditions. The conditions which affect saturation (SiCl4 concentration, flow rate, temperature) determine the number of sites on which silicon will nucleate and grow. Reaction product HCl is likely responsible for suppressing silicon growths on the oxide near exposed areas of silicon. Evidence is given that the oxide-silicon interaction occurs in hydrogen only and involves water as a transport agent. SINCE shortly after the first epitaxial layers of silicon and germanium were grown over large areas, efforts have been underway to grow selectively on specified portions of the surface. Such selective growth should be particularly applicable to monolithic integrated circuits. Usually the approach has been to use a mask to delineate the desired area,'-7 but the VLS methoda can also be used, and direct programmed atomic beam deposition has been suggested.9 The masking techniques may embody two forms: in one the mask is a material which can later be removed along with any growths attached to it; in the other, attempts are made to prevent growth on the mask, so that over a whole slice the only deposition that will occur is in the unmasked regions. The present work is concerned with only the latter case, and specifically with silicon. Joyce and Baldrey1 suggested the use of thermally grown silicon dioxide as a mask material and showed that for the proper choice of operating conditions (total flow, SiCl4 concentration, total deposition time, and temperature) spurious growth could be minimized and that if the deposition times were not too large, and the criteria not too stringent, a usable process occurred. Later Schnable et al 4 observed that after extended deposition times, during which most of the silicon dioxide became covered with growth, there was always a band of oxide around the exposed silicon area that was quite free of spurious silicon crystallites. This latter observation is particularly intriguing since it extends the hope that with proper precautions masking can be much more versatile than it presently is. EXPERIMENTAL PROCEDURE Silicon substrates oriented to within 1.5 deg of a (111) plane were prepared by etch polishing lapped

Jan 1, 1967

By R. M. Lumley, J. D. Wood

In this investigation, polyethylene terephthalate (Mylar) was coated with various thicknesses of a vapor-deposited silvel- precoat followed by a uapor-deposited zinc using several orders of- magnitude variation in deposition rate of both the silver and zinc. The grain size and resistivity of the zinc film was primarily a function of the silver precoat thickness (in the range of 0.001 to 10 average Agprecoat thickness) and a secondary function of the zinc film thick-ness. The silver and zinc deposition rates were found to have a minor effect on the characteristics of- the zinc film. Electron and X-ray dilffraction results slwwed that all zinc films exhibited a fiber texture mith the (0001) axes essentially perpendiculav to the platze of the film When coating nonmetallic substrates such as paper or plastics with zinc metal vapors, it is found that the zinc will not condense unless extremely high evaporation rates or very low substrate temperatures are used. In 1931, Fraser' reported a procedure whereby zinc could be made to condense on nonmetallic substrates by depositing a very thin precoat of silver. Utilizing Fraser's method, the ermans' developed a commercial process of making "metallized film" capacitors during World War 11. The metallizing process, which was introduced in the United States shortly after the conclusion of World War 11, became one of the first large-scale commercial applications of vapor-deposited metal films and remains one of the larger applications in the electronics industry. The process, as developed by the Germans, consisted of depositing a thin precoat of silver on lacquered, kraft paper followed by a conducting layer of zinc. The resulting silver-zinc film was used as the capacitor The term silver-zinc will be used throughout thiz paper to mean a metal film formed by an extremely thi layer of silver, 10A or less in average thickness, and a zinc film IOOA or more in thickness deposited on the silver film. ---. electrode with the lacquered paper being the dielectric. When polyethylene terephthalate was marketed by E. I. Du Pont Co. in the early 1950's under the trade name Mylar it was substituted for the kraft paper in many capacitor applications. Even though manufacture of metallized paper and metallized Mylar capacitors has been a large commercial process for many years, little information has been published about the deposition parameters. Correlating the work of others to the various effects to be expected of deposition parameters on silver-zinc films deposited on Mylar, it is expected that the

Jan 1, 1967

By J. W. Borough

THE electrical conductivity of pure copper is markedly decreased by small amounts of impurity in solution. The magnitude of this effect has been very carefully determined by numerous investigators who studied a wide variety of impurity elements. Much of this work is summarized in an excellent review by Pawlek and Reichel.' The case of zinc impurity in copper is an exception to the above in that there has been no well-documented study of the effect using high-purity starting materials. The values for the effect of zinc on conductivity, which are usually taken from unpublished work by Skowronki, indicate that zinc in low concentration has no effect whatever in lowering the conductivity of pure copper. This effect, if true, is unusual since it is generally known that even in lowest concentration, impurities exert an effect on conductivity which is proportional to the amount dissolved. It is more reasonable to suspect that in the original work on the effect of zinc some of the zinc was oxidized out of solution during specimen preparation. The following experi- and calculated d-spacings based on the unit cell dimensions of Baenziger et al. Since the single crystal studies of Baenziger et al. were limited to (hk0) and (hk 1) data, it was not possible to Compare all the intensities of the powder and single crystal patterns. However, the strongest reflections of both studies, the (321) reflection, agree very well when the appropriate multiplicity factor is used. Good agreement was also found in a number of other reflections of lesser intensity. Despite the precautions taken in annealing the U6Fe powder, an appreciable amount of UO, was detected in the powder pattern after heat treatment. The powder pattern reported by Groganoand Clews is given in Table I. Except for the 3.15A line, which is the strongest line of UO,, their pattern, as far as it goes, compares favoEably with the data from this study. Gordon and Kaufmann have reported a diffraction powder pattern purported to be U, Fe but it bears very little resemblance to the patterns of Table I. ments were carried out to redetermine the effect of zinc on conductivity using high-purity starting materials and processing conditions capable of producing oxygen-free alloys. Materials used in the experiment were ASR 99.999 pct Cu and Cumingo 99.999 pct Zn. Four 1 lb melts were prepared with identical procedure in argon atmosphere with crucibles made from Speer No. 580 graphite. The compositions were 0.0, 0.1, 0.3 and 1.0 pct Zn. Standard No. 14 wire (0.064 in. diam) was made from these melts as follows. The 1 pct Zn sample was first reduced 94 pct by cold swaging with five annealing treatments of 800o for 10 min in hydrogen between swagings, and then reduced 94 pct to the

Jan 1, 1962

By Orville A. Derby

In view of the recent important discussions before this Institute on the genesis of metalliferous deposits, certain features in the occurrence of gold which seem to be more clearly developed in Brazil than elsewhere can hardly fail to be of interest. As the observations here recorded have necessarily been of a somewhat cursory character, they will be presented in the form of brief notes, without any attempt to draw conclusions as to their genetic significance. Gold in Gneiss.—The statement made by me many years ago† that in the districts of Campanha and S?o Gongalo, in southern Minas Geraes, gold occurs in gneiss, can now be reaffirmed in the most positive manner, on the strength of a recent examination of fresh material, confirmed by the testimony of an experienced mining captain from the Morro Velho mine, who, being skeptical on this point, made a prospectingtour in the district. The specimens examined, though so far decomposed as to be readily disaggregated, were clearly of

Jan 1, 1903

By A. J. Shaler

The subject of the mechanism of sintering has received much attention in the past few years, particularly since the beginning of the series of AIME seminars in powder metallurgy of which this paper introduces the fourth. In the first of these, F. N. Rhines1 brought together and discussed the available experimental data on the sintering of pure metallic powder, and succeeded in bringing to a sharp focus the attention of workers in this field on the established observations which a satisfactory theory must explain. Several other authors3,5,6 have, in the last few years, studied the phenomena that occur when cold metallic powders, loose or in the form of compacts, are first brought to elevated temperatures. Some workers' in the field of friction have recently studied the adhesion of solid metal surfaces when they are brought into close contact. These researches have indicated that several separate mechanisms operate simultaneously, at least during the first part of the sintering process. Some of them have been called transient mechanisms4 because they are in general not absolutely necessary to sintering. Powders may be so prepared and so treated that these transient phenomena do not take place during subsequent sintering. This does not mean, of course, that their industrial and scientific importance is any less than that of the steady-state phenomena. The latter are changes that go on during sintering no matter how the powders are made or treated; they cannot be divorced from sintering. One way to analyze the process of sintering into its component parts is perhaps to distinguish between these transient and steady-state phenomena. Some of the transient phenomena have been studied in the past few years. Huttig3 has shown that, when the temperature of metallic powder is slowly raised, the following events generally occur in order: (1) physically adsorbed gases are desorbed; (2) there is an atomic rearrangement of the surface, a sort of two-dimensional "surface-reciystallization"; (3) there is a breakdown of chemically adsorbed surface compounds; (4) there is a recrystalliza-tion in the volume of the metal. All these changes are shown by Huttig and his coworkers to be completed fairly rapidly at lower temperatures than those generally used in sintering and are therefore not a part of the mechanism whereby the density of a mass of powder continues to change after long heating at an elevated temperature. But the first and third of these changes release gases in quantities which may or may not help to control the steady-state mechanisms, depending on when the voids become isolated from the outside of the compact. Among the phenomena studied by Steinberg and Wulff,8 there is the effect on sintering of residual stresses arising from the pressing operation. They found that the lateral surfaces of a green compact of iron are under a longitudinal residual tension-stress of the order of magnitude of half the yield-point for solid iron. If the outside surface is in tension, the core must be under longitudinal compression. When the compact is heated, the surface residual stress is thermally relieved first, and the compact therefore initially expands in the direction of its axis. This is a transient phenomenon, if for no other reason than the possibility of sintering unpressed powders, as demonstrated by Delisle,9 Libsch, Volterra and Wulff10 and others.1 The subject of recrystallization is dealt with further in a separate section, in view of its prominent place in sintering literature. It, too. is one of these transient phenomena. Among the steady-state parts there may be distinguished the attraction between particles and its consequences, the spheroidization of voids in the compacts, and the densification or swelling of the compact. There is considerable evidence4,7 showing that cold metallic surfaces, when brought to within a few interatomic distances of one another, are attracted to each other by forces of the order of many thousands of pounds per square inch. A calculation, discussed in greater detail in another section, shows that this force changes but slightly when the temperature of the surfaces approaches the melting point. Actual measurements of forces of adhesion of this magnitude have been made by Bradley12 on some nonmetals, but none has yet been made on cold or hot metals. This force is of sufficient magnitude to cause some plastic deformation in powder compacts, as will be shown below. A second force of steady-state nature is due to the surface tension, which probably has the same origin as the force of attraction between surfaces.164 A paper by Udin, Shaler, and Wulff1,3 gives the results of precise direct measurements of its value for solid copper. The demonstration of the tendency for the surface tension to shrink a pore was long ago given by Gibbs.17 He showed that its effect on a curved surface between two phases is equivalent to a pressure perpendicular to that

Jan 1, 1950

By F. C. Holden, R. D. Buchheit

In the course of studies made on the Ti-Cu alloy system,' particles identified visually as TiH were encountered unexpectedly in a specimen of high-purity Ti-0.8Cu alloy. The particles did not appear immediately after preparation, but following-storage in a dessicator for several days. Since the alloy had been vacuum annealed to a low hydrogen concentration (19 ppm by vacuum-fusion analysis), the appearance of the TiH particles was suspected as a surface contamination effect. A specimen of a Ti-0.8Cu alloy had been annealed 2 hr at 790°C and water quenched, to produce the single-phase equiaxed a structure. The metallo-graphic sample was ground through 600X paper, rough-polished on a high-speed wheel with a mixture of alumina and chromic acid, awLhish-polished on a slow-speed wheel. Disturbed metal layers were removed from the final surface by alternately etching with a 1 1/2 HF-3 1/2 HNO3-95 H2O solution and polishing on the slow-speed wheel with fine alumina. The final surface was swab-etched with a 1 1/2 HF-3 1/2 HNO3-95 H2O solution, rinsed in tap water, and dried in a stream of filtered air. The micro-structure, shown in Fig. 1, was composed of equiaxed a grains without any trace of second phase. After storage in a dessicator for 3 days, the appearance of small particles in the structure became evident (see Fig. 2). After 7 days of storage, the particles were more distinct, and in some grains, began to appear as elongated particles. The specimen then was etched a second time (without repolishing) to produce the structure shown in Fig. 4. On the basis of micro- structural observation, the line markings were identified as TiH; attempts to obtain diffraction patterns from the surface for positive identification were not successful. That the structure is a surface effect was demonstrated by grinding with 240X paper to remove the surface layer. The surface then was ground, polished, and etched using the procedures described previously. The same observations were made: the freshly prepared surface was devoid of any second phase, whereas the particles again appeared after several days storage. The same effect has been observed in other a-stabilized titanium alloys, including a high-purity Ti-0.20 alloy containing only 16 ppm H by analysis. The effect has not yet been observed in unalloyed titanium, nor does its appearance appear to be consistent with any particular alloy system. From these observations, it is concluded that certain a-titanium alloys are susceptible to the formation of titanium hydride at the surface of metallo-graphic specimens. The hydrogen probably is diffused into the surface from a residual film of etchant decomposition products. Estimates of the hydrogen

Jan 1, 1961

By G. S. Jenkins

The statistics set forth by Professor Mitchell in a proceding paper very carefully brought out the points that indicate that a marked amount of consideration must be given to" the haulage problem to adapt it to local conditions as encountered. Professor Mitchell's paper showed a spread of from 10 tons per man to 50 tons per man on the production crews, which spread can be recognized as entirely too large when one considers that the product is being sold at a price within very close limits. While a portion of this spread may be explained by different methods in cost accounting as to what employees are applicable to the production crew, it cannot all be blamed on an accounting method. A good portion must be explained by the improper application of equipment to the needs incurred by the local conditions. It is in an endeavor to go into this phase that this paper is given. It will be necessary to qualify the points covered in order to keep the subject from becoming too wide in scope. Along this line, conditions will be only those involved in bituminous coal mine practices and only the haulage of coal that is loaded with mobile loading machines in seams 4 ft thick and better. Haulage Methods Employed The Consolidated Coal Co. (Illinois) has been operating on a modernized basis for about 20 yr. By modernized we mean the loading of coal with mobile loading equipment. In review of haulage methods, it must be remembered that the main line electric haulage locomotive has been in service for some 40 or jo years. To augment this main line haulage, the mule did a quite satisfactory job during hand-loading days, but was later replaced by the gathering locomotive, either battery or cable-reel operated. This type of haulage was the method in common use at the time the mechanical loading of coal became of major importance and the success or failure of loading machine installations may be largely accredited to haulage facilities in the early days; that is, in the period around 1930. The Consolidated Coal Co. had its struggle with this problem beginning in about 1927 or 1928. We were somewhat fortunate in that we were already using gathering locomotives powered by storage batteries at the time we introduced mechanical loading. This meant that we did not have to spend as much time training motormen and trip riders as many mines did that utilized only mules for their secondary haulage. This was all advantage, and our efforts could be focused on ways and means of providing adequate car service to the loading machine. Like most operations, we endeavored to gear the car service to the capacity of the machine, with a large crew endeavoring to load the maximum tonnage that the machine would handle. Toward that end our first move was to install switches

Jan 1, 1949

The production of bituminous coal in Pennsylvania started a few years after that in Virginia. For forty-five years all the production came from the Pittsburgh bed, and since that time its total output in value has exceeded that of any other single mineral deposit in the world. It has been impossible to separate the outputs of the four counties producing it at that time, as none of it came from Greene County until many years later, and the figures in the first column of Table 49 represent all the coal coming from Allegheny, Fayette, Washington and Westmoreland Counties. The years prior to 1790 are grouped on account of space limitations, they were made in the same manner as the later ones. All outputs have been rounded into hundreds, or thousands of tons because their accuracy does not warrant further subdivision. All figures are net tons, and all represent production and not shipments; this distinction in the early days when transportation facilities were scarce meant a great deal. In the period 1820-1835, more coal was used in salt-making in western Pennsylvania than for any other single purpose, but not a ton of such coal was handled by any transport agency. Later the iron industry used large quantities of local coal without shipment, and other instances can be cited. Prior to 1832, the only means of shipment of coal, excepting by wagons, was by the rivers, and this tonnage was larger than is generally believed. In Table 23, all of the available data about production from the Pittsburgh bed have been shown. After 1844 the river shipments above Pittsburgh are accurately reported by the Monongahela Navigation Company, but its figures do not include tonnage loaded on the river below Dam No. 1, nor that brought down Saw Mill Run. Prior to 1844 no tonnage records were kept although the amount moved was considerable. The information about local production, not shipped, whether used domestically or for manufacturing is necessarily incomplete. Column 7, shipments by railroad, river and canal, includes the figures in column 4, and until at least 1857 are quite evidently too low. The figures in column 9 are largely estimates based on the data shown and prior to 1870, and perhaps later, are much more likely to be lower, rather than higher, than the actual ones. This table was prepared over a period of years, and as additional data were found the revisions necessary were almost always upward. Clearfield County was the next producer in the state, shipments-in small amounts going down the Susquehanna River; some were made later via the West Branch Canal. Railroad facilities became available in 1862, and the growth in production increased rapidly and steadily. All available data and the estimated totals are in Table 24. Butler County began mining a few years after Clearfield, the early output

Jan 1, 1942

By G. E. Pellissier, P. H. Salmon Cox, B. G. Reisdorf

Banding that occurred in plates rolled from the early production heats of 18Ni(250) maraging steel is described and related to the segvegation of certain alloying elements (nickel, molybdenum, titanium), the extent of which was quantitatively evaluated by means of electron-microprobe analysis. The effect of banding on mechanical properties is discussed, with particular reference to observed directional differences in plane-strain fracture toughness of plates. It is shown that banding originates as interdendritic segvegation during ingot solidification and persists in some degree through normal soaking and hot reduction to plate. The results of the study showed that heating sections of small laboratory-cast ingots at 2200°F for 4 hr was sufficient to markedly reduce microsegregation and to considerably improve mechanical properties. Hot rolling of 7-in.-thick ingot sections to 1/2-in.-thick plate effected a similar reduction of microsegregation, but resulted in even greater increases in ductility and toughness than that obtained by homogenization treatment alone. DURING the past few years, considerable attention has been directed towards the low-carbon, high-alloy maraging steels and in particular towards the 18Ni-8Co-5Mo-0.4Ti alloy. The steels of this group, having an excellent combination of high strength and toughness, have a number of advantages over their more conventional medium-carbon low-alloy, quenched-and-tempered counterparts. In the annealed condition, the maraging steels are in the form of a ductile marten-site; aging at a relatively low temperature, typically 900°F for 3 hr, increases greatly the strength through the precipitation of intermetallic compounds. One problem in the early production heats of maraging steel was that the finished plate frequently displayed a banded structure. Previous work on other steels1-' had established that banding in wrought products is either a direct or an indirect consequence of chemical segregation, which occurs during solidification and persists to some extent through normal thermal and mechanical treatments. For example, Smith and others: in a study of low-alloy steel, were able to correlate the severity of banding in the wrought product with the degree of interdendritic segregation of nickel and chromium in the as-cast ingot. The effect of banding on the mechanical properties of steels is usually considered to be detrimental, although there is only limited evidence to suggest that a marked improvement in properties can be obtained with less heterogeneous structures. Comparison of the longitudinal and transverse tensile properties of banded and of homogenized 4340 steel showed that only the transverse ductility was improved by homogenization, but even then the improvement was not commercially significant.' Conversely, homogenization of through-the-thickness tension specimens of quenched-and-tempered steel plate, containing 1.47 pct Mn, increased the strength by as much as 10 pct and the tensile ductility by at least a factor of twos5 This improvement was related to the elimination of manganese-rich bands, which also are one of the factors responsible for cold cracking in the heat-affected zone of metal-arc welds.7 In the present study the nature and severity of banding in early commercial 18Ni(250) maraging steel plate and in laboratory-melted 18Ni(250) maraging steel plate was determined. The effects of banding on plane-strain fracture toughness and the effects of thermal homogenization treatments on the strength, tensile ductility, and toughness of 18Ni(250) maraging-steel as-cast ingots and rolled plate were evaluated. In addition, the effects of hot deformation by rolling on the mechanical properties of ingots were determined. 1) STUDIES OF BANDING IN EARLY PRODUCTION PLATE The chemical composition of the steel (A) used in this part of the investigation is shown in Table I. Banding was not clearly evident in either as-rolled or annealed* plate, but annealed and agedc** plate had a banded structure. The typical banded condition, Fig. 1, consists of layers of unetched austenite (white) and dark-etching martensite in a light-etching martensitic matrix. X-ray diffraction measurements showed that this steel contained more than 6 pct austenite. An electron-probe X-ray microanalyzer (using a focused beam of electrons) was used to determine the composition of the bands and of the material between the bands with respect to the main alloying elements— nickel, molybdenum, titanium, and cobalt. The recorded X-ray intensities were converted to concentration values with the use of a standard of similar composition. To facilitate probe positioning, all analyses were conducted on specimens that had been given a light etch. The influence of this etching on the analytical results was negligible; analyses made on the identical area before and after etching yielded essentially the same concentration values. The results of the electron-microprobe analyses at selected points revealed that the layers of austenite and adjacent dark-etching martensite contained greater amounts of nickel, molybdenum, and titanium than did the surrounding matrix, Table 11. The austenite layers

Jan 1, 1968

By John B. Hastings

Ten miles from Hartsel, near Antelope springs, in Park county, Colorado, there is a large area of unconsolidated lake-beds, which are interesting because at least a part of the lacustrine sands contains in the aggregate an immense amount of gold. During 1906, one of the arms of this dessicated lake was fairly well prospected with shafts and cuts by an Eastern company to test its value, as favorable amounts of gold had in some instances been found upon it. The claims of the company contain about 5,000 acres of the beds; bat this is only a small portion of them, a south branch from a main body, which is at least 7 miles in diameter, with other and very wide lateral gulches, paralleling the one herein described on the east and west. A certain amount of digging and sampling was done in the outside areas; but the result was evidently unsatisfactory, since the work was discontinued. This section of Colorado has not been studied geologically, and the age of the ancient lake is unknown. It is probably Quaternary. I spent two weeks on the ground, in September

Jan 1, 1909

By T. M. Allen, W. H. White

THE Greenwood-Grand Forks area of southern central British Columbia, known as the Boundary District, has a long history of mining exploration and production. At the turn of the century this was the premier copper mining camp in the British Empire, its total production amounting to some 20 million tons. Most of this ore came from the great Granby mines at Phoenix, but the Motherlode mine at Deadwood camp, 6 miles to the west, and several mines in Summit camp, 5 miles north of Phoenix, made important contributions. The large deposits were exhausted in 1918 and the district since has seen only desultory exploration and salvage operations. The orebodies are mineralized skarn zones in limestone members of a thick series of Upper Paleozoic sedimentary and volcanic strata. Chalcopyrite is the primary ore-mineral. Copper carbonates and silicates occur sparingly in outcrops, but the oxidized zone generally is very shallow. Much of the surface is mantled by glacial drift which in most places ranges in thickness from 2 to 15 ft. In some of the hanging valleys, however, the glacial drift may be as much as 100 ft thick and may assume drumlin-like forms. In 1951 an ambitious program aimed at the discovery of new orebodies and important extensions of abandoned deposits was launched by Attwood Copper Mines, Ltd. In this district so thoroughly searched by an earlier generation of prospectors, any orebody which had remained undiscovered must have little or no surface indication. Consequently, in addition to the basic detailed geological work, the program of exploration included magnetometer and self-potential surveys. Geological bets and geophysical anomalies were tested further, prior to diamond drilling, by a study of copper distribution in tree twigs and/or in the soil. The soil sampling and analytical methods used and some of the results seem of sufficient importance to warrant this paper. The authors had done some plant sampling in this and other districts, using the dithizone neutral-color-end-point method (Warren and Delavault, 1948, 1949; White, 1950),1-3 but they were unfamiliar with its soil application. Finally, after much experimenting in the field, they adopted the methods described here. These methods are not entirely original or defensible on theoretical grounds, but under field conditions of rapid sampling and analysis the results are reliable enough to be of use. Fig. 1, which shows the results of duplicate analyses of duplicate soil samples taken at 50-ft intervals across an anomalous zone, indicates the relative dependability both of the sampling and analytical methods. Sampling and Analytical Equipment A 2-ft piece of 1-in. solid drill steel, one end sharpened to a broad, conical point. The steel is marked at 1 ft from the point. A 2-ft piece of ½-in. black iron pipe, one end filed to a bevelled cutting edge. The pipe is marked at 1 ft 3 in. from the cutting end. A 3-lb hammer. A plastic or rubberized sheet about 18 in. square. Moisture-proof assay pulp envelopes. A 10-mesh seive made from window screen with the paint burnt off. A small assay spatula. A pan balance sensitive to 10 mg. Two ignition trays about 4 in. square, made of sheet iron turned up along the edges. A Coleman two-burner gasoline stove. An asbestos board about 5x8 in., used as a hot plate on the gasoline stove. A circular aluminum rack to hold 8 test tubes while refluxing (design of Almond and Morris). Pyrex Glassware Large refluxing test tubes, 25x200 mm, marked at 40 ml volume. Breakers, 20 ml. Pipettes, 1, 5, and 10-ml capacity. Graduate, 50 ml. Shaking cylinders, 100 ml, glass stoppers. Burette, 25 or 50-ml capacity, with holder. Chemical Supplies 1 N sulphuric acid. Hydroxylamine hydrochloride, solid crystals. Fisher Alkacid test paper. Copper standard solution. Dithizone standard solution 60 mg per liter. Water reasonably free of metals. Soil Sampling Method: The problem of how to take a soil sample is extremely crucial. The method outlined below, adopted after a number of tests, has the advantages of uniform pattern, uniform depth, and uniform size of sample. The area to be tested was marked off by chain and compass lines 100 ft apart, normal to the strike of possible ore deposits. Numbered stakes were set at 50-ft intervals along these lines and a soil sample was taken at each stake in the following manner. The drill steel was driven into the ground normal to the slope of the surface to the marked depth of 1 ft, moved slightly from side to side, then carefully withdrawn. The iron pipe was inserted to the bottom of this hole, tapped down to the marked depth of 1 ft 3 in. and withdrawn; the 3-in. soil plug in the

Jan 1, 1955

By J. A. Snyder, W. L. Finlay

G. Edmunds—Solid solubility is considered to be of either the interstitial or the substitutional type. Is it possible, in a binary alloy as the simplest case, that some of the solute atoms are present in the normal lattice sites (substitutionally or filling lattice vacancies) while simultaneously others are in interstitial positionss One might even ask whether a distribution of the two types may be the normal situation. H. M. Meyer—Metastable states of interstitial atoms occupying vacant lattice sites possibly occur as well as of substitutional atoms squeezed in between regular matrix positions. However (as we know since Hume-Rothery), the solute atoms choose between the two kinds of solutions; consequently, every solute will be unequivocally either substitutional or interstitial in the equilibrium state of the solid solution. M. Balicki—In view of the fact that the authors apparently correlate the analysis of the alloys at the ingot stage with the properties exhibited at the testing stage, I would like to ask whether this is a fully justifiable procedure. In other words, how good are their determinations of solute concentration for correlating them with the mechanical properties. The answer to this question may explain some of the divergencies. Assuming good enough homogenization of the samples and exact determination of mechanical properties the position of the plotted experimental points will depend solely upon the accuracy of composition determination. If this is not accurate, say due to loss or pickup of elements during processing from the ingot to the testing stage, or due to a systematic error in the method employed for obtaining solute concentration data, the points will deviate from their true position and may align themselves along a different curve than the one expected. H. V. Kinsey—We have been studying the creep-rupture properties of titanium-base alloys at 1000°F. In the course of this work, anomalies in behavior of the alloys that would suggest that the material under test was becoming stronger as the test progressed have been observed. If this was so, the most likely explanation that we could think of was that the test bars were absorbing oxygen and nitrogen from the air during the test and were thereby becoming strengthened. In an attempt to determine the strengthening effect of absorbed oxygen and nitrogen the following experiment was conducted. A length of cold-rolled titanium was supplied by the E. I. du Pont Co. Two test bars, having a 1/4 in. diam gauge length, were prepared from this material. One bar was tested in the as-received condition. The second bar was heated in air at 1550°F for 100 hr and subsequently air cooled prior to testing. A testing temperature of 1000°F was employed. The results of these tests are tabulated in table 11. In the author's opinion, is it reasonable to assume that the bar that was exposed to air at 1550°F for 100 hr was stronger because it absorbed oxygen and nitrogen from the air during this heat treatment? W. L. Finlay (authors' reply)—Direct experimental evidence for or against Mr. Edmunds' interesting suggestion will probably never be available. It seems possible, however, that mixed interstitial-substitutional solid solution might well occur with interstitial elements. The less likely possibility of interstitial solution of a normally substitutional element like copper in aluminum was recently discussed at length by the

Jan 1, 1951

By M. C. Flemings, T. S. Piwonka

Pore formation is examined analytically in cellu-larly solidified single crystals, in cylindrical castings of pure metals and alloys, and in unidirectionally solidified castings. Effects are considered of fluid flow. dissolved gas, and surface tension. Experimental results show that flow through a partially solid "mushy" aluminum alloy obeys relations similar to those applicable for flow through other types of porous beds. Flow rate is proportional to the square of the fraction liquid (fL) for fL less than 0.3. Results indicate models chosen for mathematical description of pore formation in alloy solidification are valid. ONE of the solidification variables which is influential in determining mechanical properties of castings and of wrought material produced from cast ingots is porosity. This porosity may result from shrinkage, dissolved gases, or a combination of both, and may take the form of either macroscopic pores in localized areas of the casting or microporosity evenly distributed throughout large areas of the casting. In alloys which freeze over a range of temperatures some microporosity is generally found after solidification. There has been much discussion as to whether the micropores are caused primarily by shrinkage, by gas, or by a combination of both.'-3 There has, however, been little experimental or analytical work performed to delineate the relative contributions of shrinkage and gas in causing microporosity or to quantitatively describe the influence of processing variables on microporosity. Porosity other than microporosity (e.g., center line shrinkage) has also received only limited quantitative treatment.495 The aim of this work is to examine analytically the general problem of pore formation in solidification and to perform limited confirmatory experiments. Consideration is first given to shrinkage porosity in pure and nearly pure metals (shrinkage in cellular growth, centerline shrinkage in cylinders). Next, a discussion is given of formation of shrinkage-caused microporosity in unidirectional solidification and in "mushy" solidification. Finally, influences of dissolved gas and surface tension on microporosity are examined. Numerical results are given for aluminum and an aluminum alloy. Typical examples of microporosity are shown in Figs. 1 to 3, for 1) cellularly solidified aluminum, 2) sand-cast aluminum alloy, and 3) low alloy steel. SHRINKAGE POROSITY IN PURE AND NEARLY PURE METALS 1) Cellular Growth. In cellular freezing of an impure liquid, liquid grooves may exist over a considerable length of the growing crystal.6 The cross-sectional area of the grooves decreases with increasing distance from the cell tips; the root of the groove is blunt if the liquid at this point reaches eutectic composition. As a result of volume contraction during solidification, flow occurs down the groove, parallel to the growth direction; hence, there must be a pressure drop from the groove entrance to points within the groove. The geometry of the groove is simplified to that of a circular cylinder of radius r and length L, Fig. 4, L » r, and a simple and useful limiting case is obtained. This is that, in the circular cylinder freezing at constant velocity, the pressure at the root of the groove is lower than that pressure at radius r in grooves of other geometries where r decreases continuously to a lower limit at L. As discussed below, a pore resulting from a given pressure difference

Jan 1, 1967

Discussion of the paper of DORSET A. LYON and ROBERT M. KEENEY, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin. No. 92, August, 1914, pp. 1791 to 1800. LAWRENCE ADDICKS, Chrome, N. J.-I read this paper for the first time this afternoon, and it is really worthy of a much more careful reply than I can make with such a short time to consider it, but I just want to say that I differ with Dr. Lyon in his premises and conception of what happens in a refining furnace. He cites steel as an instance where the production of special grades justifies the high cost of power in an electric furnace, and goes on to say the same will be true in the case of copper, for the reason that you will get a better quality of product. I don't think you will get a higher grade of copper,. or a better conductivity, as I will explain in a moment. The cost of fuel in the Eastern plants is somewhere between 30c. and 40c. per ton of copper refined, and, if my memory serves me correctly, in an open-hearth steel furnace it is something like $1.25, so it is evident that steel could be handled to better advantage than copper on the basis of fuel. Now, taking the Great Falls plant to compare with is not quite fair, because that plant operates under peculiar conditions. The furnaces are relatively small; the coal is very bad and is very high in sulphur. No one would think of using a coal with 3.6 per cent. sulphur were anything better available. Due to these conditions, the amount of slag is inordinate, it being quoted as 3.5 per cent., and it is necessary to use lime, as there is a tendency to have troubles from arsenic owing to the very high current density used. I think he has taken about as hard a case as he could pick out. Now as to the conductivity of copper, my own idea about the reason that melted copper does not give as high a conductivity as pieces drawn directly from a cathode, or native copper, is that in the latter case the impurities are present as a mechanical mixture, while after melting they are chemically combined with the copper, which is a very different condition. Further, it is necessary to take the sample from a relatively smooth and consequently pure part of the cathode, as otherwise it would not draw. The same with the mass of copper; you pick out a good solid part of the copper, which is not representative. In fact, the refiners have all found they could not take fair samples of cathodes for a chemical analysis. It is always customary to use wire-bar copper -for the purpose of sampling, and the impurities are several times as great as shown by samples taken from .the cathodes. I think if we examine all of the examples he has given of cases where copper is higher in conductivity, it will fit with that explanation. For example, the Elmore process is a direct electrolytic deposit. Incidentally, at the present time there are a number of ex-

Jan 12, 1914

By G. F. Sager, B. J. Nelson

Magnesium alloy forgings offer higher and more uniform mechanical properties than heat treated magnesium alloy castings and are used principally for light weight parts that may be stressed in fatigue or subject to impact loads, or where space limitations do not permit the use of the necessarily bulkier magnesium alloy castings. Compositions and Properties of Magnesium Forging Alloys The nominal compositions and properties of the principal commercial magnesium forging alloys are given in Table 1. The two that are most commonly used are AMC58S and AM65S. The former has the highest strength and is, therefore, employed for heavy duty applications. However, the forging of this alloy and of AMC57S ordinarily requires the use of slow speed hydraulic presses. The forging alloy AM65S combines good, although somewhat lower, mechanical properties with excellent forging characteristics. This alloy can be forged on hammers, upsetters, rolls, and mechanical presses, as well as on hydraulic presses. These characteristics make it particularly useful for many applications. Manganese Segregation in AM65S The alloy AM65S contains 5 pct tin, 3 1/2 pct aluminum, and a small amount of manganese, the manganese being added to insure satisfactory resistance to corrosion. Some manganese segregation was occasionally encountered in this alloy. In many applications, such segregation is of no particular consequence, but when forgings are acid dipped prior to the application of various chemical coatings, the segregated particles of manganese constituent may stand in relief. The resultant surface roughening may impair appearance and is undesirable in forgings employed in the textile industry, where very smooth surfaces are essential to avoid the catching and breaking of fine threads. An effort was therefore made to determine the cause of manganese segregation in this alloy and find a method for its elimination. Radiographic examination of a series of cast ingot sections and extruded samples of the AM65S type having manganese contents ranging from zero to about 0.7 pct revealed no appreciable manganese segregation when the manganese was less than about 0.4 pct. A small amount was observed with a manganese content of 0.46 pct and considerable with manganese contents of 0.6 pct or higher. Attempts to eliminate the manganese segregation by variations in the melting and casting conditions were unsuccessful and it soon became apparent that the trouble was attributable to the fact that the manganese contents that caused segregation were in excess of the amounts that would remain in solution at temperatures encountered in the melting and/or casting operations prior to the complete solidification of the ingots. A knowledge of the amounts of manganese that would be soluble in molten alloys of the AM65S type at various temperatures was obviously desirable. The liquid solubilities of manganese in binary Mg-Mn alloys and in Mg-Al-Mn and Mg-Zn-Mn alloys have been determined by Tiner and others,* but no data on the solubility of manganese in molten magnesium alloys containing tin and aluminum are given in the literature. For this reason, an investigation to determine the solubility of manganese in a magnesium alloy containing 5 pct tin and 3.5 pct aluminum (AM65S type) was undertaken.

Jan 1, 1950

By J. P. Martin, A. H. Geisler, J. H. Crede, E. Both

The investigation of a 50 pct Co alloy was undertaken to determine whether there was any direct correlation between the structure and properties of Co-Fe alloys which were given various magnetic heat treatments. The magnetic anisotropy and texture of the 0.002-in. cold-reduced 98 pct material tend to decrease and change in nature with increasing temperature of the recrystallization anneal. Annealing samples in a magnetic field had little effect on either the magnetic properties or texture. However, cooling them in a magnetic field greatly improved their magnetic properties. THE beneficial influence of a magnetic field applied during the heat treatment of certain soft magnetic materials has been known for a long time. Early work showed that the presence of a magnetic field of a few oersteds during the heat treatment of Fe-Ni alloys will cause a large increase in maximum permeability. A pronounced increase in the residual induction which is produced by the magnetic anneal causes the hysteresis loop to approach the shape of a rectangle. Such results are beneficial since the desired properties are high permeability, high induction at maximum permeability, high residual induction, and low coercive force. More recently Libsch and coworkers1 studied the effect of magnetic annealing on the hysteresis properties of a series of Co-Fe alloys prepared from powders. They observed good response for the 35 and 50 pct Co alloys but little response for the 42 pct Co alloy. They pointed out that this was somewhat surprising since the 42 pct alloy has a high linear magnetostriction and zero crystal anisotropy and similar conditions in Fe-Ni alloys give excellent response to magnetic annealing. They found optimum properties to be at the 50 pct composition with residual induction, Br = 19,000 gauss and coercive force, Hc = 0.68 oersteds after the magnetic anneal. Before the magnetic anneal these values were B, = 12,600 gauss and Hc = 1.15 oersteds. The optimum treatment consisted of cooling from above the y-a transformation temperature to 900°C in a field of 20 oersteds, holding 11/2 hr at 900°C, then cooling at a rate of 20° to 25°C per min in the field to below 230°C. Cooling rate mainly affected coercive force with the value decreasing from 1.09 to 0.88 oersteds as the rate was increased from 3° to 48°C per min. Cooling from 1020" to 900°C in a field followed by further cooling to 230°C without the field gave properties decidedly inferior to those for samples annealed with the field applied throughout the cooling. They concluded that to get the best properties the samples must be cooled in a field to a threshold temperature above which the alloy is plastic enough to be affected by magnetostriction. In this respect the holding temperature must be high enough so that the alloy exhibits good plasticity to permit the optimum orienting of magnetic domains by relaxation of magnetostriction. In contrast, the holding time was of less significance for there was little improvement when the time exceeded 1/2 hr. The improvement in properties effected by magnetic annealing has usually been attributed to the establishment of a domain texture caused by the "freezing in" of magnetic strains. On the other hand, Smoluchowski and Turner2,3 apparently found that a magnetic field applied during recrystallization could alter the crystal texture. If this effect is real, improved properties would also be expected when

Jan 1, 1954

By L. H. Wolfe, J. O. Thieme

The tensile and shear strengths of frozen soil and the compressive strengths of ice and frozen soil were measured These tests showed that the strength of ice and of frozen soil increased as the temperature was decreased. A method is presented for the measurement of thermal conductivity and specific heat of earth and ice. Using the parameters thermal conductivity, specific heat and density, the thermal diffusivity was calculated. Results of thermal property tests establish water as the major variable contributing to thermal property values. INTRODUCTION During the last few years, a considerable interest has developed in underground storage of cryogenic liquids such as liquid natural gas. Because of its economy and safety, underground storage is being used. Before underground caverns could be seriously considered, however, the strength and thermal characteristics of the soil had to be obtained. Methods are presented herein for measuring tensile, compressive and shear strengths, specific heats and thermal conductivities. The tests were performed on two soils at temperatures from ambient to -195C. Because it is difficult to find data in the literature that pertain to a particular soil, ice was used to evaluate some of the experimental procedures. Some of our ice data are compared to the published values. PHYSICAI, PROPERTIES SOIL SELECTION AND SAMPLE PREPARATIONS The physical and thermal tests were performed on recompacted samples of two typical soils that might be encountered in underground caverns: a gray, fire clay that had been pulverized and mixed with water into a pliable mud; and a brown, sandy silt that was dug from a dry river bank and subsequent1y mixed with tap water. The moisture content of the test specimens was 17 to 22 per cent (based on the wet weight of the soil). This amount of water nearly saturated the silt, but the clay was well below the saturation point. The soils are partially described by the sieve analyses (Fig. 1) which show the particle size distribution of the coarser than 44 micron portion of the soils. The curves also show that approximately 75 per cent of the clay and 20 per cent of the silt are finer than 44 microns. The particle size seems to affect some of the physical properties, and the finer than 44 micron portion is important in the thermal conductivity test. Physical specimens were cut with a bandsaw from frozen blocks of the soil. The specimens were then sanded and kept frozen until after they were tested. They were stored at the approximate test temperature for several hours. Then, to equilibrate the samples to the test temperature, they were stored at the temperature at least an hour before they were tested. TEST EQUIPMENT An Instron, which is a constant speed gear-driven instrument, applied force to the samples and drew stress-strain plots of the test. All of the samples were strained at 0.02 in./min. All of the physical tests were conducted in a temperature cabinet that controlled the temperature to 1C. TENSILE STRENGTH Briquette or "dog-bone" shaped tensile specimens were pulled with suitably shaped jaws. This shape of specimen, which is usually used for tensile tests of concrete, is satisfactory for testing frozen soils except that the samples tend to

Jan 1, 1965

By F. A. Crossley

The key to disagreements between Blackburn's findings and mine is the word equilibrium". My work attempted to define the equilibrium diagram of the titanium-rich end of the Ti-A1 system. It can readily be shown that Blackburn's conclusions are based primarily on the examination of structures substantially removed from equilibrium. The diagram presented in Fig. 16 is properly labeled a "phase diagram". However, it appears that Blackburn either does not understand or does not accept the difference between "phase diagram" and "equilibrium diagram" as defined in the Metals Handbook.17 The conflict lies not in Blackburn's data but in his interpretation of it, and his use of "transformation", "phase diagram", and "equilibrium diagram" as synonymous terms. I share his view that the light microscope is much inferior to the transmission electron microscope for the study of transformations; but this fact does not render the light microscope useless or untrustworthy. The difficulties experienced with the Ti-A1 system have not been due to the limitations of the light microscope, but rather to the extreme sluggishness in achieving equilibrium at temperatures below 1000° C. Were it not for the light microscope employed with polarized light, the twin phase syndrome' might still be unrecognized and, as a consequence, still adding to the confusion of Ti-A1 investigations. (Ref. 1 should read ... Contract No. N161-25952 ... vol. 236.) Other, more sophisticated techniques, including electron transmission, simply confirm the erroneous tentative conclusions drawn from observations of structures due to the twin-phase syndrome. By the standards of most of the investigations of the Ti-A1 systems, seven of the fifteen compositions investigated by Blackburn were seriously contaminated with oxygen. The writer has found that 0.1 wt pct 0 shifts the a + Ti3A1 boundary to 1 at. pct lower A1 content at 700°C. At constant aluminum content, this corresponds to a temperature shift of the boundary of +25°c.18 Blackburn advises that the first group of alloys contained 0.1 to 0.15 wt pct 0, bur he does say whether the analyses were performed on as-received material or on specimens in their final state of heat treatment. This is especially important considering the 20-mil-thick starting materials. If specimens had been annealed in the two-phase a + 6 region it would have provided an indication of the final degree of oxygen contamination since up to about 12 at. pct A1 the boundaries of this region are well-defined for low-oxygen alloys. Blackburn questions the capability of light microscopy in determining phase boundaries in the Ti-A1 system. I submit that the a/a + Ti3A1 boundary in Fig. 1 of Ref. 1 over the composition range from 10 to 18 at. pct A1 was determined by dilatometry and supported by electron diffraction. Specimens of alloys containing 8, 10, 12, and 14 at. pct A1 were aged at 550°C for 1000 hr (under stress of 5000 psi to accelerate the tendency to equilibrium) and then fractured in tension at room temperature. Collodion was applied to the as-fractured (unetched) surface and, when stripped, carried away particles identified by electron diffraction as Ti3A1. Perhaps Blackburn will explain why these electron diffraction data were ignored. At this time, a technique for revealing or indicating

Jan 1, 1969