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By R. M. Caves

High-purity dense tungsten coating is obtained by means of a modified de Boer-van Arkel iodide process using tungsten bromides. The all-glass reaction system is pumped, baked, and sealed (pinched-off) at about 10-7 mm Hg pressure. The bromides then formed in situ are decomposed, depositing tungsten on heated tungsten surfaces. Heating of the specimen is done inductively in a novel arrangement that avoids electrodes of glass-to-metal seals. The tungsten, deposited at specimen temperatures from 2000° to 2800°F and bulb (halide) temperatures of 225" to 725°F, was adherent and uniform, and ranged in thickness to 1/8-in. REFRACTORY metals are of interest at NASA for use in hypersonic aircraft, in rocket engines, and in other thrust devices where very high temperatures are encountered. Tungsten, with a melting point about 6100° F, is potentially very useful for some of these applications. Considerable research on tungsten and its alloys is currently being conducted at the NASA Lewis Research Center. In this tungsten research program, there is need for a method of depositing high-purity, nonporous tungsten coatirlgs. Metallurgical bonding of the coating both to itself and to the substrate is required. In addition, it is necessary to be able to deposit thin, uniform coatings on substrates of a variety of shapes and sizes for laboratory test purposes. A survey of the methods previously used for depositing tungsten coatings indicated that none would likely meet these requirements for high purity, good uniformity, and high density except thermal decomposition of the halides. The method for coating that was selected for investigation was the thermal decomposition of tungsten bromide. This is a variation of the van Arkel and de Boer iodide process established years ago and recently reviewed.1,2 This process is applicable to the transition metals in general. More recently, the application and techniques were extended with chlorine3 and fluorine,4 and included the coating of tungsten. This is believed to be the first report on the use of the bromide for tungsten coating. Bromine was chosen over the other halogens because it promised a lower temperature for tungsten

Jan 1, 1962

By Paul L. Hunter

Nearly 2000 people are employed at Kennecott's Chino Mines Division, which recently completed its 50th year as a leading copper producer. Chino operates an open pit mine at Santa Rita, N.M., and a reduction plant, including mill, power plant, and smelter, at Hurley, N.M. The property mines 66,000 tons of copper ore and materials per day. There have been safety and industrial health programs at Chino for a number of years, but in 1955 these procedures were reorganized on a more active basis. The following discussion evaluates the progress made during the 1955-1958 period.

Jan 6, 1960

By E. C. W. Perryman

The recovery of X-ray line broadening, hardness, and electrical resistivity from cold worked AI-Mg alloys has been investigated. The results, together with those from density measurements, suggest that magnesium atoms freeze in the excess vacancies formed by cold working, and that this affects the climb of dislocations during the recovery process. PREVIOUS work1, " has shown that while 1 pct Mg increases the activation energy for recrystalliza-tion, it decreases the activation energy for the recovery of mechanical properties and decreases the subgrain size both after cold working and annealing. A similar result has been reported by Varley2 for an A1-2 pct Mg alloy. With plastic deformation at high temperatures, McLean and Farmer' and Rachinger have found that magnesium appears to retard the motion of dislocations and, furthermore, they find little or no effect of magnesium on the size of subgrains formed during high temperature deformation. In view of the apparent contradictions as to the effect of magnesium on subgrain size, the recovery process in Al-Mg alloys has been investigated more thoroughly by studying the annealing out of X-ray line broadening, hardness, and electrical resistivity from alloys cold worked at room temperature. Material Used—The chemical analyses of the alloys are given in Table I. Fabrication—The material used was cold rolled 20 pct at room temperature, the grain size prior to the last cold rolling operation being similar to that used in previous work; i.e., 230. The experimental procedure for annealing, determination of X-rav half-veak breadth. hardness measurement, electEica1 resistivity, and density and metallographic examination was exactly the same as previously described." Variation of X-Ray Half-Peak Breadth with Annealing Time—Isothermal annealing curves at 100°, 200°, and 250°C were obtained for material cold worked 20 pct. The half-peak breadth of the (333) Ka, line directly after cold working is shown as a function of magnesium content in Fig. 1. Only with the 2.87 pct Mg alloy was overlapping of the a, and n.. reflections observed to any appreciable extent. To separate these, Rachinger's method' was used. Typical isothermal annealing curves are shown in Figs. 2 and 3 for 100" and 200°C, respectively. These curves are similar to those obtained previously for super-purity aluminum except that the

Jan 1, 1957

By Gunnar Thaning, Borje Bjorkvall

At LKAB Central Division for Metallurgical Research at Malmberget, Sweden, fired pellets are examined in respect to mechanical and reduction properties. The paper deals with descriptions of the test methods. It also involves the rationale for the choice of these tests. Their correlation to the blast furnace operation will be examined. The mechanical tests used are the ISO-tumbler test and the cold compression strength test. Concerning the metallurgical properties, experiments have shown that some superbasic pellets in particular have different disintegration properties in different temperature ranges. Pellets which have favorable reduction properties when tested under isothermal reduction at high temperature may disintegrate to a large extent under low temperature reduction. This is also valid for some types of acid pellets. Consequently, it was found to be necessary to determine the reduction strength both at high and low temperatures. In the low temperature range, the disintegration is measured by tumbling the pellets in soft reducing conditions at 600°C in a modified Linder test equipment. The high temperature reduction strength is determined under load in the Burghardt-Grebe equipment. However, in order to get more information of the high temperature strength, LKAB intends to introduce a softening test. The tendency of high temperature disintegration will also turn up in the swelling test. The swelling properties are examined according to a procedure developed at LKAB. In this test the pellets are subjected to free swelling without mutual contact. The reducibility of the pellets is recorded in the swelling test.

Jan 1, 1974

By H. Reiss

The zone-melting process in which redistribution of solute in a solid bar is effected by the passage of a molten zone is considered mathematically. Simple approximate techniques are developed for computing the manner in which redistribution occurs as molten zones continue to pass. The introduction of the "zone-melting flux" provides valuable insight into the nature of the phenomenon, as well as a central mathematical theme in terms of which the process can be discussed. Curves are presented for typical and general cases. AN extremely efficient purification technique was described recently by Pfann.1 Known as zone refining, it consisted of the slow passage of a series of molten zones, produced by external heaters, through a long solid ingot of the substance to be purified. Equations were given for the maximum separation attainable, and a numerical computation method was described for obtaining the concentration in the ingot after a given number of zone passes. The present paper offers an interpretation of the physical nature of zone melting in terms of a transport process in which formal diffusive and convec-tive flows occur. This interpretation, in addition to providing insight into the physical nature of the process, also provides a basis for its mathematical treatment. From this basis, useful equations are developed for the solute concentration in the ingot as a function of the number of zone passes. These are applicable particularly where large numbers of passes are necessary and where numerical computational methods might be laborious. All considerations will deal with the limiting form of the process, described by Pfann,' in which: 1—Diffusion in the solid is considered negligible. 2—Mixing in the liquid is supposed, complete. 3—The distribution coefficient, k, measuring the ratio (at equilibrium) of solute concentration in the solid to that in the liquid is supposed, independent of composition. In general, this paper will be concerned with a bar of uniform (actually unit) cross section, ex- tending in the x-direction from x = 0 to x = L, where L may be infinite. Zone melting is a transport process, and as such must admit of interpretation in terms of a flux of transported quantity. However, the progress of operation is not measured in units of time but in terms of the number of completed zone passes. Consequently, the zone-melting flux will be a rate, per unit pass, rather than per unit time. The description of this flux and the examination of its properties is given below. Zone-Melting Flux Fig. 1 represents an intermediate stage of the nth pass. Concentration C is plotted against distance, x. The molten zone with its back at the point x and front at x + I moves in the direction indicated by the arrow. As it moves, it leaves behind the nth

Jan 1, 1955

US Tin Mission To Study Costs in Far East A move to obtain adequate supplies of tin at prices the United States is willing to pay was initiated when the interagency tin mission left for the Far East. The Mission, which includes representatives of the Reconstruction Finance Corporation, State Department, Defense Minerals Procurement Agency and the Bureau of Mines will go to Indonesia and Malaya. The primary purpose of the mission, according to officials, will be to study tin production costs, not to negotiate for the purchase of tin. The mission will be prepared to enter into negotiations, if the Far Eastern producers are amenable. The United States withdrew as a large-scale buyer of tin some months ago in protest against what it considered exorbitant prices being charged in the Singapore market. Subsequent attempts to negotiate for a steady tin supply at what this country considers reasonable prices have been unavailing. The U. S. is prepared to enter into a two or three year contract with the price of tin somewhere between $1.00 to $1.12 per lb. The decision to abstain from the market has not yet put a squeeze on U. S. supplies. Substantial quantities of tin still are coming in from Malaya under an old contract.

Jan 12, 1951

By AIME

THE history of the Mine La Motte area covers a greater period of time than any other mining operation west of the Mississippi, for it was almost exactly four centuries ago that the white man first visited the region. In May 1541 a few men from the party of Fernando de Soto traversed the place looking for silver which they understood the Indians had found in the vicinity. Some historians say that De Soto himself visited the place sometime later. No other white man came through again until the early 1700's. In 1712 King Louis XIV of France granted to Antoine Crozat a charter for transacting all business and government in the vast domain of the New Continent stretching from the Gulf of Mexico northward indefinitely. This

Jan 1, 1947

By S. E. Bronisz, Dana L. Douglass

a Uranium was deformed by cold rolling, and the effects of this plustic deformation on the microstruc-ture of the metal were observed by the technique of transmission elecbon microscopy. The recrystalli-zation of selected cold-wmked samples was also studied by this method. The samples were prepared for examination by electrolytic thinning in a standard metallographic electrolyte which has not been previously reported as being used in producing thin foils of uranium. The microstructural changes observed in the a uranium were generally similar to those seen by optical microscopy. The changes in the microstructure of a uranium following cold work and recrystallization treatments have been the subjects of several studies employing optical and X-ray techniques.12-19 These studies indicated that twinning was the redominant mode of deformation at room temperature20 and that the regions of high energy associated with the deformation twins were preferred sites for the initiation of recrystallization.15,18, Recently several workers have prepared thin foils of uranium suitable for examination by transmission electron microscopy.'-lo The foils thus prepared have been used to study fission fragment damage; a particular dislocation reaction,' and gas precipitation." At this laboratory the microstructural changes occurring during the cold working and recrystallizing of a uranium samples have been studied by using transmission electron-microscopy techniques. The foils used in this work were electrolytically thinned in a polishing bath not reported previously in the literature as being used for this purpose. EXPERIMENTAL PROCEDURE The uranium used in this investigation was depleted a uranium sheet 4 mils thick. The results of a spectrochemical analysis of this material are shown in Table I. The as-received uranium was cut into strips, 1 in. wide by 5 in. long, and annealed in vacuo at 600°C for 2-1/2 hr. The resulting microstructure consisted of relatively uniform, equiaxed grains having diameters of 10 to 50 p. Cold Working. The cold-worked samples were prepared by rolling several of the annealed uranium strips to various thicknesses. The strips were reduced 3.5 ± 0.5, 6.0 ± 0.6, 10.0 ± 0.5, 19.5 ± 1.0, and 28.5 ± 2.0 pct in thickness. It was not possible to achieve these reductions with a single pass through the rolling mill, so the strips were turned end for end during the rolling procedure. The cold-rolled strips were stored in dry ice until samples from them could be thinned and examined (within 24 hr after rolling). Annealing. The samples used in studying the re-crystallization behavior of a uranium were obtained by annealing sections of the strips which had been reduced 10.0 and 28.5 pct. These samples were sealed in evacuated Pyrex capsules and were annealed in a tube furnace at temperatures from 200" to 600°C and for times from 1/2 to 2 hr, see Table l. Thinning: The samples from the rolling and heat treatments were prepared for examination in the electron microscope by electropolishing in a bath composed of 25 g chromic acid, 133 ml glacial acetic acid, and 25 ml water. This electrolyte has been used and recommended for preparing specimens for optical metallography It was necessary to mask the edges of the sample with a stop-off paint in order to prevent preferential attack in these areas. The paint used was made by dissolving polystyrene in benzene. The electrolytic cell consisted of a cylindrical stainless-steel cathode placed in a beaker containing the electrolyte, with the sample as the anode positioned at the cell axis. The temperature of the electrolyte was held below 15°C by cooling with liquid

Jan 1, 1963

By AIME AIME

MESSRS. BURT and Shockley and others have been for three years urging upon the Institute the matter of simplified spelling. The Institute endeavors to be progressive in the matter of spelling and. is in cooperation with the national body which has this in hand and which has its principal office in New York. Our spellings are changed as fast as-good usage will permit (so it seems to the Board of Directors) and the national body, which is the real representative of the simplified spelling interests, deems that the Institute is making real progress, although not quite as fast as extremists would wish. In January, 1919, Mr. Shockley sent out letter ballots which created a misconception in the minds of many members, who received the impression that the communications came from the Institute instead of from a small group of members. As a result of this propaganda 163 proposal-ballots were sent in to the Institute divided as follows: Yes ?114 No ?20 Negative letters ?9 Split ballots ?20 Total ?163 The total membership at this time was about 7200. The disgusted members would not vote.

Jan 1, 1920

By G. W. Preckshot, J. W. Gorman

MOLTEN metals offer an excellent medium for the study of molecular diffusion and interphase transfer. In the absence of intermetallic compound formation, solutions of molten metals are solutions of elements. Therefore, complicating factors such as molecular structure, dissociation, association, polarization, and so on, are generally absent. Further, metals remain in the liquid state over a wide range of temperature. Thus, the effect of temperature on transport processes can be studied in more detail. Although some data are available for the diffusion of metals in the molten state at high temperatures,"""".'!' the most useful and accurate data are those for the diffusion of various elements in mercury at room temperature. The effective radius of diffusion for the various elements in mercury may be calculated from the Stokes-Einstein relation.'-These calculated radii are compared with the atomic and ionic radii calculated from X-ray data on crystals." The effective radii of diffusion of the alkali and alkali-earth metals correspond to those of the neutral atom; those of cadmium, silver, lead, zinc, thallium, bismuth, and tin correspond to ionic radii; and those of copper and gold indicate larger radii due to association with mercury or more likely, faulty diffusion data. Independent evidence"' supports the notion that alkali metals are uncharged in amalgams. The concept of metals moving free of their conductance electrons in the liquid state has been discussed by Eyring, et al,'" in connection with studies on the viscosity of pure molten metals. Considering the approximate nature of the tabulated atomic and ionic radii and the variance in the diffusion measurements, the application of the Stokes-Einstein equation to the diffusion of metals in mercury gives gratifying results. It is noted that a number of these metals have article radii eaual to or less than those of the solvent mercury.".'*,"' Soba1,'" sing the inaccurate Roberts-Austin20 data, indicated that the effective radius of diffusion might well be a function of temperature. Additionally in studies of mass transfer between phases, many conflicting opinions have been expressed concerning the assumption of equilibrium at the interface." ,","," The results of the present work on the diffusion of solid copper in molten lead throws light on the tempera- ture variation of the diffusion radius as well as the extent of the interfacial resistance. The theoretical background and experimental procedure are presented here in detail. Results on other systems will be presented in subsequent papers. Nomenclature The following nomenclature is used in the paper: A—cross-sectional area of diffusion column, sq cm C, C,—concentration of solution and saturated solution respectively, g per cc D,D'—-diffusivity, sq cm per sec e—Naperian base h—ratio, k/D k—mass-transfer coefficient, cm per sec L—diffusion column length, cm n—series index q—flux, g per sq cm-sec r—radius, cm or A R—-gas constant t—time, sec T—temperature, K V—volume, cc w—weight of copper-lead alloy on copper cylinder WT—-total copper transferred to lead diffusion, column, g Z—distance from top of diffusion column, cm 2'—distance from copper-lead interface, cm (2' = L-2) u,,—roots of diffusion equation Mathematical Apparatus The model shown in Fig. 1 applies to the diffusion of solid copper into molten lead. Here Fick's first law may be written where all terms are defined in the nomenclature. It is assumed that the volume of the lead column is constant. This is justified since experimental densities compared favorably with calculated densities based on perfect interstitial mixing. Thus there is no counter diffusion of lead. It is clear that 2 in Equation [I] should be measured relative to the interface which moves relative to the diffusion cell but not to the liquid phase. Hence, the frame of reference is the plane of the copper-lead interface. The diffusivity calculated at constant volume, D", is that defined by Hartly and Crank" and is designated herein as D. No Interfacial Resistance—The two situations of the presence and absence of interfacial resistance will be treated. The simplest is the latter which re-

Jan 1, 1959

By Ove Sandberg, Olav Bowitz

The operational characteristics of the Soderberg vertical spike anode are briefly discussed stressing the importance of the flow properties of paste in the fluid zone, the thermal shrinkage in the carbonizing zone, and the surface disintegration in the consumption zone. The requirements for paste recipe and binder quality are combined with design and operation of cell. A low temperature susceptibility of viscosity and low thermal shrinkage of paste together with a low microporosity of the binder coke are important properties. PRACTICAL application of Soderberg's idea of a selfbaking carbon electrode proved successful just before 1920. Shortly after, experimental work was started with the aim of developing a continuous electrode that could be adopted as anode in aluminium reduction cells. The intermittent operation of a large number of small prebaked anodes made the idea of developing a continuous anode for electrolytic production of aluminium especially tempting. Moreover, the electrode consumption in this process, even on a theoretical basis, is very high. Many installations were carried out in the 1930's and during the Second World War. During the tremendous post-war expansion of the aluminium industry, the Soderberg electrode has been steadily more widely adopted. Thus, today more than 60 pct of the Western World's output of aluminium is produced in cells with selfbaking anodes, see Big. 1. The quality of the anode paste of Sfiderberg elec- trodes is considered a major factor influencing the specific carbon consumption. The purpose of this paper is to survey the fundamental requirements which must be met in order to obtain good anode operation. We have limited this paper to a discussion of Elektrokemisk's research on the vertical spike type anode. I) FUNDAMEKI'TALS OF ANODE CARBON PERFORMANCE A) Brief Introduction. The only practical method for producing a conductive carbon anode of the size required is to form and carbonize a mixture of a carbonaceous binder and a precalcined dry aggregate coke. In the Soderberg electrode, the forming and carbonization take place in the electrolytic cell

Jan 1, 1962

By V. H. Wilhelm

WITH rapidly diminishing oil reserves: a great percentage of which are uneconomical at present prices, some of the existing methods of development and production will have to undergo radical re- visions to meet the changes continually taking place in the petroleum industry. Imagination in an engineer is a great asset. The fancy of today is found to be the realization of tomorrow, and with this thought in mind, there is here presented a more or less imaginative picture which, to my mind, has a meritorious basis. Directed drilling has reached a stage of accuracy sufficient to allow the prediction that this art will be used in the future development of oil structures, especially those \\,it11 thin sand bodies 'and steep dips. Directional drilling in a number of fields in California has gratifying results. Wells which practically laid pipe lines through the oil sands have enjoyed a greater drainage radius with a consequent greater initial and cumulative production. In one field where the vertical thickness of sands was approximately 550 ft., wells drifting at an angle as great as 55 deg. fro111 vertical had over 1100 ft. of perforated pipe in contact with these sands. These wells were, and are, remarkable for their great initial pro-

Jan 1, 1936

James GayleY, New Pork City (communication to the Secretary*) :—The main thing that is sought after in this matter is that all purcliases shall be made by analysis. This is done already in special lines, as in the manufacture of various grades of steel in which phosphorus, silicon and sulphur are specified within narrow limits, and I quite agree with Mr. Cook that specifications, which are over-rigid in unessential particulars, should be avoided, as they defeat their own purpose because unreasonable requirements permitting no variation are practically not fulfilled, and it is impossible to specify grade

Jan 1, 1905

By A. H. Daane, R. L. Myklebust

The yttrium-manganese system has been investigated by thermal, metallographic, and X-ray diffraction methods. There are three intermetallic compounds present: YMn2 which melts congruently, YMn4, which undergoes syntectic decomposition, and YMn,, which undergoes peritectic decomposition. The compound YMn4 is ferromagnetic at room temperature with a Curie temperature of 214°C. There are eutectics at 25.2, 60.9, and 82.0 wt pct Mn which melt at 878°, 1100°, and 1075°C, respectively. Crys-tallographic data are given for YMn4, and YMn12 . The terminal solid solubilities are low. In a general program of study of yttrium metal in this laboratory some alloy systems of this metal with elements of the first transition period have been examined. This work was originally instigated by experiences in cladding yttrium with jackets of some protective metals such as Inconel for high-temperature service in air.' In some cases a low-melting phase was observed to form between the Inconel and the yttrium resulting in failure of the samples. In characterizing this reaction, a survey was made of the systems of yttrium with chromium, manganese, iron and nickel,, and it was found that a eutectic was formed between these metals and yttrium on the yttrium-rich side of the system. This present study of the Y-Mn system was carried out to examine in more detail the alloying nature of yttrium, and to correlate trends that have been observed in previous related studies. It was observed by Voge13 that in the systems of lanthanum, cerium, and praseodymium with each of the metals in the first transition series, the tendency to form compounds diminished in the order nickel, cobalt, and iron while no compounds were formed with manganese, chromium, or titanium. Beaudry and Daane4 observed a similar behavior in the systems of yttrium with some members of the first transition series except that the tendency for compound formation was greater. Both the Y-Ti5 and Y-Cra systems consist of simple eutectics, while in the Y-Fe,7 Y-CO, and Y-Ni4 systems, there are four, eight, and nine compounds, respectively. In addition to the above trends, the similar atomic radii and electronegativities of yttrium and thorium invite a comparison between their alloying behaviors with a common element such as manganese. In crys- tallographic studies, Florio et al.' have identified three intermediate phases in this system which are ThMn2, Th6Mn23, and ThMn,,. Gschneidner and Waber10 have examined published information on alloy systems of the rare-earth metals and have correlated this information with current alloying theory. From their study, they predicted that the Y-Mn system would contain one intermetallic compound. On the basis of this prediction, the trend in the alloying behavior of yttrium with the elements of the first transition series and the alloying behavior of thorium with manganese, one might expect from one to three intermetallic compounds to form in the Y-Mn system. A consideration of Hume-Rothery's rules of alloying based on size-factor, electronegativity, and valency suggested a small terminal solubility and possible compound formation. The present study was undertaken to confirm these predictions of low terminal solid solubility and compound formation and to establish the general alloying behavior of yttrium with manganese. EXPERIMENTAL Materials. The manganese used in this investigation was obtained from the Foote Mineral Co. as electrolytic plates of 99.9 pct stated purity; the yttrium metal was prepared in this laboratory. Table I gives the analyses of these materials. For the solubility studies at the yttrium-rich end of the alloy system, distilled yttrium, whose major impurity was 200 ppm Ti, was used. Preparation of Alloys. The alloys were formed by comelting the two metals in an are-melting furnace under an atmosphere of argon. The buttons thus formed were inverted and remelted three to five times to promote homogeneity. Due to the high vapor pressure of manganese, it was assumed that the weight lost during are-melting was all manganese. This assumption was based on the very good agreement observed between calculated compositions and chemical analyses of several alloys. The compositions of the dilute alloys used for solid solu-

Jan 1, 1962

By E. H. Hamilton

THE furnace on which the following investigation was based had dimensions 48 by 160 in., and was in continuous operation during the three days of the test. The average charge consisted of PER CENT. LB. PER HOUR Bed ore?14.5?2,980 Roast from Dwight-Lloyds?44.5?9,160 Siliceous ore?3.5?720 Iron flux?2.1?430 Battery plates?0.5?103 Lime rock?23.9?4,925 Briquettes?4.0?825 Scrap iron?2.1?430 M. P. slag?4.2?865 L. P.speiss?0.7?142 Total 100.0 THE furnace on which the following investigation was based had dimensions 48 by 160 in., and was in continuous operation during the three days of the test. The average charge consisted of PER CENT. LB. PER HOUR Bed ore?14.5?2,980 Roast from Dwight-Lloyds?44.5?9,160 Siliceous ore?3.5?720 Iron flux?2.1?430 Battery plates?0.5?103 Lime rock?23.9?4,925 Briquettes?4.0?825 Scrap iron?2.1?430 M. P. slag?4.2?865 L. P.speiss?0.7?142 Total?100.0?20,580

Jan 1, 1924

Executive Committee. CHESTER F. LEE, Chairman. C. R. CLAGHORN, Vice-Chairman. WC. BUTLER. M. K. LODGERS. Joseph DANIELS, Secretary-Treasurer. Meeting, Jai. 25, 1913.-Dean Milnor Roberts read a paper on The Equipment and Curricula of the College of Mines, University of Washington.

Jan 4, 1913

By J. W. Schroeder

SEAMLESS pipe, the product produced from piercing a solid round billet of steel by the Mannesmann process, was first produced in the latter half of the 19th century, the Mannesmann machine having been patented in 1885. The products of other processes also have been termed seamless pipe; for example, the cylindrical section produced by "cupping," which consists of forming a cup from a flat plate or disk and further elongating the cup into a tube by passing it through a set of reducing dies. The purpose of this paper is to discuss some of the more important metallurgical factors and their relationship to the economical production of seamless pipe produced by the Mannesmann piercing process. The first seamless tube plant in America was established at Shelby, Ohio, in 1891, and was employed in the manufacture of bicycle tubing. For a number of years the bicycle industry was the only user of seamless tubing, and this tubing was produced by hot-rolling pierced billets imported from Europe and finishing on the cold drawbench. At the turn of the century, the automotive industry was responsible for an increase in the demand for seamless tubing. The growth of this industry was the dominant factor leading to the phenomenal growth of the petroleum industry, which in turn created a tremendous demand for seamless pipe. In addition; the old lapweld iron boiler tubes for stationary and locomotive boilers were replaced gradually by seamless tubes. Since 1929, the production of seamless steel pipe and tubes has increased over loo pct. In 1929, 1,459,9031 net tons of seamless pipe was produced, including both hot-finished and cold-drawn material, as compared with 3,087,3122 net [ ] tons in 1948. Table I gives the distribution of seamless pipe by classes for 1948. METALLURGICAL PROBLEMS From a metallurgical standpoint, the production of seamless pipe has presented many problems. Practically every type of steel, carbon and alloy, with the exception of the superalloys developed during World War II, has been pierced and rolled successfully into tubing. This includes bessemer, open hearth, by the stationary and duplex processes, and electric steels. The range of sizes produced is no less staggering to the imagination, when it is considered that the hypodermic needle, which is 0.016 in. diam with a wall thickness of 0.004 in., and pipe for gas or oil transmission lines, with a 26 in. OD, are both seamless tubes. Between these extremes, the range of diameters and wall thicknesses meets most present-day demands for seam-

Jan 1, 1951

By M. E. Hassan, J. C. Calhoun, R. F. Nielson

An apparatus was constructed for the measurement of inter-facial tensions over a range of temperatures and pressures. This apparatus utilized the pendent drop method, and resembles in construction similar apparatus recently described in the literature and in use in some petroleum research laboratories. The interfacial tensions of benzene, propane, n-pentane, n-hexane. n-octane. and iso-octane against water were measured at temperatures ranging from 26" to 82" C and at pressures ranging from 1 to 204 atm. Values of interfacial tensions for the henzene-water system and their variations with temperature and pressure are generally in good agreement with value? of previous investigations. The data in all cases showed a slight decrease of interfacial tension with pressure at constant temperature in the range studied. The effect of pressure became less as the pressure was increased, with an indication of a reversal of the effect at higher pressures. There was a decrease of interfacial tension with temperature at constant pressure in all cases, as would normally be expected. This rate of decrease became greater the higher the temperature. A general equation is presented for the interfacial tensions as a function of presPurp and temperature over the range studied, and the constants calculated for each system. A definite trend was found in the effect of molecular weight on the interfacial tension at a given temperature and pressure, for the homologous series from propane to n-octane. Data for n-decane from the literature fitted well into this trend. INTRODUCTION It has been recognized for many years that surface forces play an active part in the production history of an oil reservoir as well as in determining the amount of unrecoverable oil. The magnitudes of these forces are governed by the values of the interfacial tensions. These vary greatly with composition, pressure, and temperature. The effect of composition is greater than that of pressure and temperature over the ranges normally encountered. In fact, because of the variety of compounds present in a crude, no attempt has yet been made to correlate crude composition with its surface tension or with its interfacial tension against water. The amount of dissolved methane greatly affects the surface properties of an oil, and there are "surface-active" compounds in crudes which have a much greater effect on boundary tensions than do equal amounts of hydrocarbons. The purpose of the present work was partly to contribute data that would eventually be used in correlations applicable

Jan 1, 1953

By J. J. Jonas, J. L. Uvira

Equipment was constructed which permitted the hot compression of 99.8 pct Armco iron and 2.8 pct Si steel at constant true strain rates of 0.05 to 1 per sec over the temperature range 600" to 1000°C. A maximum true strain of 1.9 could be attained, followed by immediate quenching or by isothermal annealing. True stress-true strain curves were obtained, and the steady-state flout stress, a, strain rate, i, and temperature, T, were found to fit the following expression: The constants A, a, n', and AH were determined for the two ,materials. The activation energies obtained for Arrnco iron and silicon steel are 66 and 80 kcal per mole, respectively, and approximate those for seu- diffusion and for creep. This indicates that hot compression is a diffusion-controlled thermally activated process. THE hot compression of iron and steel is usually carried out in the austenite temperature range,1"7 as this is the one of greatest interest with respect to industrial hot working. However, a disadvantage of testing in the austenite range is that the hot-worked structure is destroyed by the phase transformations taking place during cooling. The present study was therefore carried out in the ferritic temperature range, and the hot-worked substructures were preserved by rapid quenching after deformation. The substructural results will be described in a separate paper, and the present communication is restricted to the strain rate/stress/temperature relationship observed during hot working. The results of hot-compression testing are usually given in the form of true stress/true strain curves, with a different curve for each temperature/strain rate ~ornbination.',~,~ Sometimes simple algebraic equations are fitted to the curves, so that certain extrapolations or interpolations can be performed.1'2'5 These equations are, however, devoid of mechanistic interpretations. The present study was undertaken to show that hot compression can be described by an equation of the type used in creep studies. That is, it will be shown that the temperature dependence of the strain rate in hot working is well-represented by an Arrhenius term, with an activation energy similar to that for creep. Also it will be seen that the stress dependence of the strain rate is similar to that for creep EXPERIMENTAL METHOD AND MATERIALS The investigation was carried out with the following three ferrous materials: 1) Armco iron; 2) Armco iron with 0.26 pct Mn; 3) 2.8 pct Si steel. The first two materials were utilized for investigations performed in the temperature range 600" to 800°C; the last one was used for tests at temperatures from 600" to 1000°C. The materials were of commercial purity,* as shown in Table I. Cylinders of five different sizes were prepared by strain annealing. The resulting mean grain diameter was 3 mm in the 1-in. Armco iron and 2 mm in the other sizes and grades. Different ratios of diameter/height were used to enable the determination of the coefficient of friction. The specimen faces were provided with concentric grooves, which acted as lubricant holders during compression, as recommended by English and ~ackofen' and others.2'9 Powdered glass lubricants were applied to the samples before hot compression to decrease friction and barreling, following the practice of previous investigator~.~~~~~~~~ Different mixtures of glass powder were used for each temperature, after the determination of suitable compositions by experiment.'' Equipment for Hot Compression. Hot-compression tests were carried out on an adapted 150-ton vertical hydraulic extrusion press and also on a modified high-temperature creep machine. The modified extrusion press was used for temperatures up to 800°C. The following items were added to the press: a) a high-temperature furnace with built-in upper and lower platens; and b) a transmission assembly, which permitted the attainment of logarithmically decreasing crosshead speeds. These accessories are described in detail in Ref. 11.

Jan 1, 1969

By H. H. Podgurski, Hsun Hu

Large cryslals of high-purily iron (99.996+ pcl) cannot be obtained by the usual strain-ameal technique. Repealed phase transformation by thermal cycling prior to crilical deformation improves the capabilily of cryslal growith but fails to yield satisfactory crystals. Imperfect columnar crystals can be produced by the phase-transition method. The addition of a small amounl (0.005 wl pet) of nilrogen IT was reported'-4 that for metals of very high purity the usual procedures of the strain-anneal technique fail to produce large crystals. This was eliminates practically all the difficulties in crystal growth by the normal strain-anneal procedures. An actual example is presented, showing that most parts of a strip have been converted into a large crystal by this method. The addition of nitrogen, which can be removed from iron with less difficulty, is believed to be more desirable than carbon additions for the same purpose. thought to be due to the strong tendency for recovery in the high-purity metals: hence the critically strained matrix undergoes polygonization instead of recrystallization upon annealing for crystal growth. Talbot1,2 succeeded in overcoming this difficulty by adding 0.03 to 0.04 pct C to high-purity iron before critical deformation. followed by annealing in hydro-

Jan 1, 1965