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By J. D. Hanawalt, C. E. Nelson, J. A. Peloubet

The subject of the salt-water corrosion resistance of magnesium alloys is somewhat like that of the pitting of stainless steels, in that it involves a relatively small. percentage of the applications but receives a much greater proportion of the publicity. Actually magnesium alloys are in use in many exterior applications as well as interior, with no trouble from corrosion. Magnesium and its alloys have a striking stability against atmospheric attack, being far superior to iron. Specimens exposed unprotected to atmospheric weathering for Io Years show only a superficial surface-film formation. The basic nature of magnesium and of its important alloys is that they are also resistant to the attack of salt water even in an unprotected state, giving substantially no loss in weight after one year of alternate immersion in 3 per cent NaCl solution (Fig. 1). This basic behavior is often masked because of the extreme sensitivity of these alloys to certain impurities and combinations of impurities. It is known, and the subject of increasing emphasis, that higher purity leads generally to greater stability for many materials, non-metallic as well as metallic. However, a review of the literature on the corrosion factors in magnesium alloys shows that almost all researchers worked with base metal in which metallic impurities varied in uncontrolled amounts. The major factor, that of metallic impurities, Probably greatly overshadowed the effects of minor ones such as flux inclusions, nonmetallic impurities, porosity, metallographic state, which these researchers presumed to study. In the present investigation the first observation of interest is that whereas magnesium of commercial purity (99.9 per cent pure) has a corrosion rate in alternate immersion in 3 per cent NaCl solution at room temperature of anywhere from 5 to Ioo mg. per sq. cm. per day, the corrosion rate of high.purity magnesium is 0.15 ± 0.05 mg, per sq. cm. per day. The principle followed in the experiments was to add to such base magnesium other elements, singly and in inin in controlled and known amounts and to observe the corrosion behavior of the resulting alloy. These experiments show the existence of what may be called tolerance limits" of magnesium and some of its alloys for certain impurities. The extremely small percentages of impurities involved and the sharpness of the corrosion discontinuities appear to be quite unpredictable, In order to carry on this work, it was necessary to develop an analysis technique suitable to the problem. In some cases it was necessary quantitatively to analyze impurities to less than 0,001 per cent. The experimental data to be presented are based on observation of about 5000 alloy specimens and on more than 50,000 quantitative analyses. while the primary purpose of this paper is to present the experimentally obtained data on corrosion rates as a function of composition, and particularly to demon-

Jan 1, 1942

By W. J. Babyak

The habit planes for hydride precipitation in large grains of alpha zirconium and Zircaloy-4 were determined in specimens containing 161 and 136 ppm hydrogen, respectively. In zirconium, the hydride platelets precipitated on various pyramidal planes inclined to the basal plane at angles ranging from 10 to 50 deg and 75 to 90 deg. Hydrides were most frequent at inclinations of about 20 deg and 90 deg. In Zircaloy-4, hydride plates were inclined to the basal plane at angles vanging from 5 to 25 deg with the predominant inclinatioiz equal to 12 deg; no platelets were found near the prism plane position. In both zircoinium and Zir-caloy-4, hydrides were principally, but not exclusively, parallel to (1011) type planes. When the Zircaloy-4 gmins were subjected to tension stresses of 12,100 psi and 19,400 psi during hydride precipitation, the hydride habit was unchanged except that precipitation favored those habit planes which were inore nearly perpendicular to the stress direction. The stress-orientatioiz effect increased with the magnitude of the stress. THE hydride habit plane in a zirconium has been determined by several investigators. Langeron and Lehr1 in 1956 found platelets parallel to (1010) slip planes. In 1962, Westlake and Fisher2 confirmed these findings and showed that hydride precipitation on twin planes, as reported by Kunz and Bibb,3 was probably due to incomplete removal of worked metal from specimen surfaces. Secondary habit planes, ( 1011) and (1015), were also found by Westlake and Fisher under particular charging conditions where a hydride layer may have existed at the hydrogenation temperature. Most recently, walters4 and westlake5 again observed the (1010) habit exclusively in zirconium. Louthan and hgermans have reported that hydrides precipitate on various ( 101l ) and (112l) planes positioned 31.5 to 90 deg to the basal plane in Zircaloy-2. The present investigation was concerned with the hydride habit in Zircaloy-4 in relation to that in zirconium and the possible change in habit when precipitation occurs under stress. The latter consideration was prompted by the stress-orientation phenomenon originally reported by Marshall and Louthan.7, 8 I) EXPERIMENTAL Materials and Specimens. Chemical analyses of all materials are given in Table I. The zirconium specimen was a 1 by 4 in. section cut from wrought crystal bar that was hot-rolled at 790°C to 0.300 in. and cold-rolled to a final thickness of 0.095 in. All surfaces were mechanically polished and then chemically polished with a solution of H2O, HNO3, and HF (10:10:l by volume) prior to annealing. Grains as long as 0.25 in. were grown by thermally cycling the specimen three times (in 10-5 mm Hg vacuum) between 825" and 1000°C at approximately 125°C per hr. The specimen was isothermally annealed at 825°C for 24, 40, and 120 hr after each cy-

Jan 1, 1968

By Cyril Wells, Robert F. Mehl

The practical importance of a knowledge of the rates of diffusion of carbon and of alloying elements in steel has often been pointed out.l,13 This importance lies chiefly, though by no means only, in the study of carbufizing and in the study of reactions involved in the eutectoid inversion in steel. The present paper is one of a series in which the rates of diffusion of carbon and of alloying elements in ?-Fe and their mutual effects are measured with precision. The present paper reports the results of measurements of diffusion coefficients D of manganese in ?-Fe over wide ranges of temperature, and concentration, and of the effect of carbon and impurities and of grain size upon these diffusion coefficients.‡ Data on the rate of diffusion of manganese in ?-Fe have been reported by Fry2 and by Paschke and Hauttmann.3 Claussen4 calculated the diffusion coefficient D from Fry's data as 3 X 10-10 sq, cm. per set. at 960º, which will be shown to be incorrect by many orders of magnitude. Paschke and Hauttmann gave a rough value of 9.6 x 10-8 Sq. cm. per set. at 14000. Neither of these workers considered the variation of D with concentration and with temperature, and neither studied the effect of carbon. Method and Materials Method.—The method employed is identical with that used earlier.5 Owing to the volatility of manganese and the consequent loss of manganese from the outer surfaces of the welded diffusion bars, these surfaces were discarded. The diffusion anneals were performed in argon, except One (test 18) in which hydrogen was employed for purposes noted below. The temperatures reported are accurate to about 3" and constant within 1°C; the diffusion times are reported to the nearest half hour. The specimens were furnace-coo1ed after the diffusion ation, at about 2° per min. Layers, usually 0.004 in. thick, parallel to the welded interface, were machined from the specimens after the diffusion anneal and analyzed for manganese to 0.I Per cent Mn; the distances of these layers from the interface was measured to ±0.0002 in. The concentration-penetration curves obtained were analyzed by both the Grube and the Matano solutions.8 The D values calculated by these two methods do not differ appreci000. The Grube solution was used except in tests in which the effect of concentration upon D was greater than so per cent; in such cases the Matano method, which explicitly provides for the variation of D with concentration,' is the more reliable. In general, the number of layers machined from the zones of variable composition were large enough to permit the use of the average layer composition as that of the center of the layer. In 3 of the 3' tests, however, this is not justified, and the D values

Jan 1, 1941

By Cyril Wells, Robert F. Mehl

The practical importance of a knowledge of the rates of diffusion of carbon and of alloying elements in steel has often been pointed out.l,13 This importance lies chiefly, though by no means only, in the study of carbufizing and in the study of reactions involved in the eutectoid inversion in steel. The present paper is one of a series in which the rates of diffusion of carbon and of alloying elements in ?-Fe and their mutual effects are measured with precision. The present paper reports the results of measurements of diffusion coefficients D of manganese in ?-Fe over wide ranges of temperature, and concentration, and of the effect of carbon and impurities and of grain size upon these diffusion coefficients.‡ Data on the rate of diffusion of manganese in ?-Fe have been reported by Fry2 and by Paschke and Hauttmann.3 Claussen4 calculated the diffusion coefficient D from Fry's data as 3 X 10-10 sq, cm. per set. at 960º, which will be shown to be incorrect by many orders of magnitude. Paschke and Hauttmann gave a rough value of 9.6 x 10-8 Sq. cm. per set. at 14000. Neither of these workers considered the variation of D with concentration and with temperature, and neither studied the effect of carbon. Method and Materials Method.—The method employed is identical with that used earlier.5 Owing to the volatility of manganese and the consequent loss of manganese from the outer surfaces of the welded diffusion bars, these surfaces were discarded. The diffusion anneals were performed in argon, except One (test 18) in which hydrogen was employed for purposes noted below. The temperatures reported are accurate to about 3" and constant within 1°C; the diffusion times are reported to the nearest half hour. The specimens were furnace-coo1ed after the diffusion ation, at about 2° per min. Layers, usually 0.004 in. thick, parallel to the welded interface, were machined from the specimens after the diffusion anneal and analyzed for manganese to 0.I Per cent Mn; the distances of these layers from the interface was measured to ±0.0002 in. The concentration-penetration curves obtained were analyzed by both the Grube and the Matano solutions.8 The D values calculated by these two methods do not differ appreci000. The Grube solution was used except in tests in which the effect of concentration upon D was greater than so per cent; in such cases the Matano method, which explicitly provides for the variation of D with concentration,' is the more reliable. In general, the number of layers machined from the zones of variable composition were large enough to permit the use of the average layer composition as that of the center of the layer. In 3 of the 3' tests, however, this is not justified, and the D values

Jan 1, 1941

By A. A. Watts, R. I. Jaffee, F. C. Holden, H. R. Ogden

Hypoeutectoid Ti-Cu alloys are responsive to heat treatment, and considerable variation of mechanical properties may be produced by transformation of the ß phase. Control of cooling rate, isothermal transformation, or quench tempering determine the transformation structure and properties. The transformation products are similar to those of carbon steel. THE equilibrium diagram for the Ti-Cu system has been studied by various investigators, and the most recent diagram is that determined by Jou-kainen, Grant, and Floe.' The titanium-rich portion of this diagram is reproduced in Fig. 1. The alloy compositions and annealing temperatures used in this work are shown. The Ti-Cu alloys containing up to 17 wt pct Cu are representative of an active eutectoid alloy system. Joukainen et a1.l have stated that ß phase cannot be retained on quenching and this has been confirmed in the present work. The similarity between the Ti-Cu system and the Fe-C system is evident and, as will be shown later, many of the transformation products appear to have similar microstructures. Heat treatments in this program were designed to produce the structures of primary interest for study and determination of mechanical properties. Experimental Procedures Preparation of Alloys: Five ½ lb ingots, ranging in composition from 0.8 to 6.83 pct Cu, were prepared by double arc melting in an atmosphere of high purity argon. Titanium melting stock was obtained from high purity iodide titanium, and copper additions were made from copper wire clippings. Segregation was reduced by inversion melting, in which the once-melted ingots were inverted in the crucible and remelted. The double-melted ingots were forged at 1600°F to ¾ in. diam rods, with both heating and forging operations being carried out in air. Surface scale was removed by grit blasting and grinding, after which the forgings were vacuum annealed at 900°C. The alloys then were swaged to ¾ in. diam rod at 750°C and test specimens were cut from this material. The vacuum annealing operation was to remove dissolved hydrogen, which is commonly present in the iodide titanium as-received. Although vacuum fusion analyses were not obtained for all these alloys, past experience indicates that the 6 hr treatment with a limiting pressure of 10- to 10-5 mm of Hg is sufficient to reduce the hydrogen level to 10 to 30 ppm. Vacuum fusion analysis of the 0.8 pct Cu alloy showed 19 ppm of hydrogen. In addition to the five hypoeutectoid alloys, three 15 g ingots were prepared with nominal copper additions of 9, 10, and 11 pct. Fabrication procedures were similar, except that these alloys were rolled to 0.040 in. sheet. Microstructure specimens only were obtained. Table I shows analyzed compositions and fabrication temperatures for these alloys. Heat Treatments: All heat treatments were made in potentiometer-controlled, resistance-wound tube

Jan 1, 1956

By L. J. Dijkstra, R. J. Sladek

IN earlier work the effect of manganese on the general behavior of nitrogen in iron was the subject of a careful examination by Fast.' Part of the investigation was made, in collaboration with one of the present authors (L.J.D.), by using the internal friction method. This technique, which has been described elsewhere,' showed some significant changes in the properties of Fe-N alloys by the addition of a small amount of manganese namely: 1—Under standard conditions the maximum of the nitrogen peak in pure iron appears around 20 °C and the half width is about 27 °C. By addition of 0.5 atomic pct Mn a general broadening of the internal friction peak occurs. The half width is increased by about 9°C. Moreover, a shift of the maximum of about 5°C toward a higher temperature takes place, Fig. 2. 2—The precipitation of nitrogen from the supersaturated solution, measured, e.g., at 200 °C, was inhibited by the addition of the amount of manganese given in effect 1. The broadening of the nitrogen peak was confirmed in more recent work3 on samples which were prepared from Westinghouse Puron iron. The effect of manganese on the rate of precipitation, however, was much less striking than in the earlier work' based on Philips high purity iron. Theory To explain the first change in properties just referred to, effect 1, the following two assumptions were made:' First, every manganese atom in sub-stitutional solid solution creates around it six interstices located between an iron and a manganese atom, as is evident from Fig. 1. These interstices, conveniently called Fe-Mn interstices, have for nitrogen a free energy level which is AG* lower than the normal Fe-Fe interstices between two iron atoms. For such low concentrations of manganese as 0.5 atomic pct, the possibility that two manganese atoms will be nearest neighbors can be disregarded. Second, it is assumed that in addition to the normal relaxation time TFe at least one new relaxation time, Mn, Fe, enters in the phenomena which is associated with the elementary diffusion jumps between a Fe-Mn interstice and an adjacent Fe-Fe interstice. Fig. 1 gives schematically the free energy for a nitrogen atom as a function of its position along the line ABC. A tentative analysis of the nitrogen peak in a 0.5 pct Fe-Mn alloy based on these assumptions has been made in Fig. 2. The dotted curve with a maximum at 22°C is caused by jumps between Fe-Fe interstices, the dotted curve with maximum at 32°C by jumps between an Fe-Mn and an Fe-Fe interstice. The two effects added together give the dash-dot internal friction curve for the alloy. In the following these two components will be referred to as the normal peak at 22°C and the abnormal one. (The small secondary peak at

Jan 1, 1954

By C. W. Covington, H. C. Cook, J. F. Libsch

Sputtered aluminum thin films were prepared in each of two conventional bell-jar vacuum systems. One system utilized an inner "getter sputtering" enclosure; the second system was a standard diode sputterirlg arrangement. Consistent and repeatable film properties were obtained in both systems provided sufficient cleanup and presputter time was allowed. The various problems associated with aluminum sputtering are discussed, with pavticular attention to the vzinimization of film contamination by outgassing and oxidation. The growth and structure of the aluminum thin films were studied with the aid of electron wzicroscopy and related to deposition rate, substrate temperature, and film thickness. The resistivity of the films was correlated to film structure and surface roughness. Resistiuities as low as 3.5 microhm-cm (2.3 x bulk resistiuity) were measured for relatively thick films (20,000). THIS investigation was undertaken to explore the problems and film characteristics associated with the sputtering of aluminum. Earlier work reported on aluminum sputtering has stressed the contamination of both the cathode and film as well as abnormally low deposition rates.' Data on sputtering yields,3 however, indicate that aluminum sputtering could be practical. Recently, it was shown by Theuerer and Hauser3 that aluminum sputtering was feasible in a conventional oil-diffusion pumped vacuum system provided an inner "getter sputtering" enclosure was employed to minimize gaseous contamination. This technique employs the getter action of aluminum to produce extremely low reactive gas partial pressures in the deposition zone. Aluminum films have already found use in solid-state electronic devices such as transistors and integrated microcircuits. To the present time, most aluminum films have been prepared by evaporation due to the ease with which this metal can be evaporated. Controlled sputtering of aluminum offers a number of advantages over evaporation, however, such as 1) manufacturing compatibility with other metals which must be sputtered, 2) better control of process variables resulting in more repeatable and uniform films, 3) generally better adhesion resulting from higher-energy metal atoms, 4) built-in material supply for continuous operation, and 5) the ability to deposit alloys. The data presented in this paper are the result of two separate studies. One study utilized a small "getter sputtering" enclosure (System A) and was concerned with the structure and properties of thin aluminum films up to about 1600A thick. In this thickness range, study of the film structure was possible with transmission electron microscopy. The second study was conducted with a conventional diode sputtering apparatus (System B) and covered $ much wider range of film thickness up to about 34,000A. Emphasis was placed on developing techniques which would extend aluminum sputtering to an existing in-line continuous deposition process.4 I) EQUIPMENT AND PROCEDURE System A. Fig. 1 shows a schematic of the "getter sputtering" inner chamber used and Fig. 2 is a photograph of this chamber mounted on an 18-in. access ring of a standard liquid-nitrogen trapped bell-jar vacuum system. This chamber was designed after a similar system used by Theuerer and auser.3 The configuration allowed the glow to emanate in all directions from the cathode. Argon (99.99') was allowed to enter only at the top of the chamber such that most of the reactive gases entering with the argon were reacted with the aluminum vapor and deposited on the chilled walls of the chamber before reaching the deposition zone. Provision was also made as shown, Fig. 1, for heating and cooling the substrate from about 20" to 400°C. Two substrate materials were used: Corning 7059 glass (12 by 12 by 0.048 in.) and carbon films about

Jan 1, 1967

By H. T. Bowman

FOR more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the 1860's it was recognized that the process would benefit by some type of instrumental control.1 However, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower's eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham3' A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient monoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. CARBON-FEO RELATIONSHIP In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by McCutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a different method than were those

Jan 1, 1942

By D. R. Pratt, R. W. Hanks

The method of Caldwell and Babbitt for detennining Bingham plastic rheological constants from engineering pipe flow data has been erroneously used in many previous applications. A reanalysis of extensive pipe flow data from the literature is performed. Critical Reynolds numbers corresponding to the laminar-turbulent transition calculated from these data are found to agree with theoretically calculated values for the entire flow range studied. Similar agreement is found for the authors&apos; own data&apos; for flow of 10 slurries between parallel plates. The Bingham plastic model is shown to be a reliable representation of the flow of non-Newtonian slurries provided it is properly applied. If the Hedstrom number He = pD2 t0/?2 > 104, then the linear approximation method of Caldwell and Babbitt is invalid for pipe flow data obtained in systems of ordinary engineering interest, and the complete nonlinear form of the pipe flow Bingham plastic equation must be used in determining rheological parameters. INTRODUCTION Many materials of engineering interest must be handled and transported as slurries or suspensions of insoluble particulate matter in a Newtonian liquid. These suspensions frequently exhibit non-Newtonian rheological behavior which is reasonably well described by the simple Bingham plastic rheological equation1 Using this particular equation to describe the laminar flow characteristics of slurries was discussed at length by Caldwell and Babbitt2-4 who considered the flow of various clay slurries and sewage sludges. The model has since been used by many others.5-7 More recently the problem of predicting the laminar turbulent transition Reynolds number for Bingham plastic fluids has been treated8 for the case of flow in pipes. This paper points out errors which have existed in the analysis of Bingham plastic flow since the work of Caldwell and Babbitt2-4 and presents a reanalysis of the laminar turbulent transition calculatiod for Bingham plastic flow in pipes. In addition, new data obtained for flow of Bingham plastic slurries between parallel plates, both in laminar flow and in the laminar turbulent transition region, will be presented and compared with the theoretical analysis of laminar turbulent transition for flow between parallel plates. THEORETICAL ANALYSIS PIPE FLOW The mathematical analysisl-4 of laminar flow of a Bingham plastic fluid leads to the following equation. where q = <v>/R is a pseudoshear rate, rw is the wall shear stress Eo = r0/rw, r0 is the yield stress and 1 is the coefficient of rigidity or plastic viscosity from Eq. 1. Caldwell and Babbitt2-4 recognized that the quartic term in Eq. 2 was small compared to the other terms whenever 5, « 1, and that for large values of 7, a plot of Eq. 2 becomes linear. The slope of such a plot with rw as ordinate is 4? and the intercept is (4/3) ro. This approximation is illustrated schematically in Fig. 1. The shaded region between the true curve and the straight-line approximation near the origin represents the contribution of the quartic term. In principle, therefore,

By John Mullen

Impingers TWO types of midget impinger apparatus are used at Climax. The Mine Safety Appliances Company&apos;s midget impinger (MSA) and the Climax Molybdenum Company&apos;s midget impinger (CMC) (Fig. I). The Leiman Brother&apos;s No. 25, positive displacement pump is used in the CMC impinger instead of the four-cylinder radial pump that is used in the MSA impinger. With the MSA apparatus it is possible to obtain the proper vacuum by adjusting the needle valve on the vacuum chamber, while with the CMC impinger the proper vacuum is obtained by varying the rate at which the pump is cranked. The Leiman Brother&apos;s No. 25 pump is built to displace 0.1 cu. ft. of air per min. when operated at 145 r.p.m. In the CMC impinger this pump is so geared that the required crank speed is approximately 59 r.p.m. Both types of impinger apparatus are equipped with a water gauge mounted on top of the case and they are calibrated and operated in reference to the gauge. The MSA impinger flasks and nozzles are used with both types. Calibrating Impingers A calibrated precision Sargent wet-test meter (Fig. 2) is used in calibrating the impinger apparatus. The apparatus is set up as for taking a sample in the field, except that the hose from the outlet side of the meter is attached to the impinger nozzle. One revolution of the large hand of the meter indicates 0.1 cu. ft. of air displaced. The impinger pump is cranked for one minute, therefore, at a rate that will cause the large hand of the meter to make one revolution. The gauge reading is noted, then the impinger is cranked at this rate for 10 min. and is checked for error. If the meter indicates that more or less than I cu. ft. of air has been displaced, the impinger must be cranked—ither slower or faster according to the error—for another 10 min. and again checked for error. This operation is repeated until the proper gauge reading for a sampling rate of 0.1 cu. ft. per min. has been determined. This gauge reading is used in all sampling operations until the impinger is again calibrated. An impinger is calibrated at least twice each week. MlCROPROJECTOR A Bausch and Lomb model B micro-projector is used (Fig. 3). It consists of a substantial metal base supporting the light source and a microscope. Illumination is provided by a Bausch and Lomb 4.5-amp. arc lamp with mechanical feed. A glass water cell filled with a heat-absorbing and color-filter solution is placed between the arc lamp and the microscope. Two types of solution have been found satisfactory— a 2 per cent solution of copper sulphate or a 2 per cent solution of picric acid and distilled water. This percentage may be varied to give the desired color to the light reflected upon the screen. Any standard microscope may be used. A Bausch and Lomb microscope with

Jan 1, 1946

NEW MEMBERS The following list comprises the names of those persons who became members during the period of Oct. 10, 1917, to Nov. 10, 1917. ABEY, HIROSHI Min. & Met. Engr.. Mitsubishi Co., Tokio, Japan. BARNETT, WALTER W., Assayer & Chem., Seoul Min. Co., Tul Mi Chung, Chosen, Korea. BATES, WILLIAM S Min. Engr., Anaconda Copper Min. Co., Butte, Mont. BENDELARI, ARTHUR E Mgr. of Mines, Eagle Picher Lead Co., Picher, Okla. BERKEFELD, PAUL C Mining Engr., 2901 Piedmont Ave., Berkeley, Cal. BILLINGS, It. S Mgr., Sheep Trail Pyramid Mines Co., Kingman, Ariz. BILLWILLER, C. J., JR Mgr. Nitrate Agencies, Ltd., Iquique, Chile. BLUM, EDWARD H., Engr., Asst., to Pres., The Atlantic Refining Co., 3144 Passyunk Ave., Philadelphia, Pa. BORDEN, GAIL, Vice-Pres. & Treas., American Safety Explosive Co., 50 East 42d St., New York, N. Y. BRESLIN, THOMAS F Min. Engr., Cebu, Cebu, P. I. BURKE, JAMES M., Efficiency Engr., Calumet & Hecla Mining Co., Calumet, Mich. CANTON, WILLIAM R Met., Nevada Consolidated Copper Co., McGill, Nev.

Jan 12, 1917

By A. J. Hatch

Recent disclosures concerning strengthening of anisotropic sheet materials under biaxial stresses are reviewed. This biaxial strengthening has been termed "texture hardening" by Backofen and is related to the normal anisotropy parameter, R. Measurements of R made on three annealed titanium alloys indicate a Ti-4Al alloy will have the greatest potential for texture hardening, followed in order by Ti-5Al-2.5Sn and Ti-6Al-4V. Relative to sheet texture, a review of the deformation mechanisms in titanium alloys would indicate that a preferred orientation for "texture hardening" is where the (0001) pole is normal to the sheet plane. This was confirmed by determination oj (0001) pole figures for the above three alloys. High R values are related to pole figures with (0001) normal to the sheet plane, whereas low R values are related to pole figures with (0001) split in the transverse direction from the sheet normal. PUBLISHED work by Backofen et al. 1 and Hosford and Backofen2 based on hill&apos;s&apos; mathematical theory of yielding in anisotropic metals has indicated that significant strength advantages under biaxial stresses are possible in hcp alloys, provided an ideal (0001) [1010] sheet texture exists. This tendency to strengthen under biaxial stresses has been termed "texture hardening".1 It can be quantita- tively characterized by a strain-ratio parameter, R, where R may be determined from the ratio of natural width strain to natural thickness strain as measured on a uniaxial test specimen cut parallel to the rolling direction. If R is greater than 1.0, then strengthening under biaxial tension would be predicted. Considering the a titanium alloys which have an hcp crystal structure, Williams and Eppelsheimer4 have reported that commercial-purity grades deviate from the ideal (0001) sheet texture mainly in an approximate 30-deg rotation of the basal plane, toward the transverse sheet direction. However, McHargue et a1.5 have shown that the angle of rotation of the basal plane is sensitive to alloy content. In particular, a titanium alloy with 3.8 pct Al was reported to have the ideal (0001) [1010] texture after cold rolling. Additionally, Backofen et a1.1 using plane-strain compression tests have reported R values greater than 5.0 for the commercial 0 alloy Ti-5A1-2.Sn (110-AT). In view of these findings, a program was initiated to further determine the potential of commercial Ti-5A1-2.5Sn and an experimental Ti-4A1 alloy with respect to "texture hardening". Also, because of its wide commercial use, Ti-6A1-4V was included in the investigation. BIAXIAL-STRESS THEORY FOR ANISOTROPIC MATERIALS Backofen ef al.,1 based on the mathematical theory of Hi11,3 has introduced the concept of "texture hardening". In this work, it was shown that possi-

Jan 1, 1965

By R. N. Orava, L. A. Rice

One of the difficulties encountered in the preparation of titanium specimens for transmission electron microscopy is the formation of a surface hydride phase during the thinning operation at ambient temperatures. This necessarily destroys contrast, obscures features of interest, and often leads to misleading results. By cooling the polishing solution to temperatures below 0°C this problem has been overcome in the past.&apos; However, since the cooling procedure is somewhat inconvenient, a technique was developed at this laboratory for thinning titanium at room temperature. The material examined was A-70 grade commercial-purity titanium purchased from the Crucible Steel Co. of America. The mechanical and thermal treatments, described elsewhere,* yielded a recrystallized grain size of 4 to 5 p. A slice, 0.5 mm thick and 1.5 mm wide, was cut from a bulk specimen2 using a diamond cut-off wheel. The sample was then coated with paraffin wax. Two concentric holes, about 0.03 in. in diam, one at each broad face, were scribed through the wax to the surface of the metal. Subsequent polishing for several minutes resulted in a preferentially thinned or "dimpled" region. Thereafter, the wax was removed and the entire specimen polished to the point of breakthrough at the base of the dimple. Polishing was effected chemically in a solution comprised of 30 pct HF and 70 pct HN03 by volume, kept at room temperature (20" to 25OC). The specimens were mounted in a stereo holder and examined at 100 kv in a Philips l00 B Electron Microscope. A micrograph from a foil prepared in this way is shown in Fig. 1. Several points are noteworthy. This electron micrograph shows neither evidence for the formation of a hydride phase due to specimen preparation nor, moreover, any obvious surface contamination in electron-transparent areas of a freshly prepared foil. Localized variations in foil thickness observed in some specimens seem to be a characteristic of this chemical polish but do not seriously detract from foil quality. With care, the lifetime of a good specimen exceeded 2 hr in the beam. On the other hand, the exposure of a sample to air at atmospheric pressure, when still warm from the beam, clearly resulted in the deterioration of a formerly clean area just previously in the field of view. An example in Fig. 2 of a contaminated region reveals features, and "spots", not unlike those observed in much purer material by Yamane and Ueda. Consequently, one can conclude that: 1) titanium can be thinned satisfactorily in a solution at room temperature for transmission electron microscopy; 2) large-scale precipitates, >50A in diam, are absent in commercial-purity, recrystallized, furnace-cooled, A-70 titanium containing about 3800 wt ppm interstitials and the same amount of iron; 3) care must be taken not to attribute surface contaminants to precipitates. The authors are grateful to the Franklin Institute for financial support and permission to publish.

Jan 1, 1967

By R. G. Vardiman, M. R. Achter

THERE has been interest recently in the conditions under which dislocation pipe diffusion may be observed. In order to extend the measurements to temperatures below Tm/2, where pipe diffusion becomes more important, a chemical sectioning technique was developed for silver single crystals which makes possible the removal of layers of 100A or less. The procedure is briefly as follows. Silver single crystals of 99.995 pct purity were cut in the form of discs t by 4 in., electropolished, and electropolated with Ag110 to about 1000A thickness. The thickness was determined by calibrating the activity with the weight of heavier platings, up to 10,000A. Both diffused and undiffused samples were sectioned in a two-step process. Reaction with a solution of iodine in alcohol formed a thin, even layer of AgI, which was then dissolved in a KCN solution. The reaction rate of the iodine solution varied slightly over a period of time, so that the thickness of the stripped layers, while quite even and regular for a given specimen, ranged from 65 to l00W for different specimens. This variation was checked by using a thickly plated standard with each run. Layer thickness was determined from undiffused samples by the point where the layer activity drops to half the maximum. This maximum intensity also provides, with appropriate corrections, the initial concentration per layer co. Because of the small penetration distances, it is necessary to use the exact solution of Fick&apos;s law for a source of finite thickness.&apos; For a plating of thick- where c is the concentration at depth x. flj the error function, D the apparent diffusion coefficient, and t the time. The diffusion coefficient was obtained from the concentration-penetration data by extrapolating to x = 0 where c/co = erf h/2(Dt)1/2 Enough points were taken to impart confidence in the accuracy of the intersection, generally about ten layers. Four temperatures were used as in Table I. For best accuracy, t and h were chosen to give values of the parameter (Dt)1/2/h between 1.0 and 1.7. A typical concentration-penetration curve is shown in Fig. 1. The diffusion coefficients calculated from Eq. [I] are plotted in Fig. 2. For comparison, the high-temperature data of Tomizuka and sonder 2 which go down to 630°C are plotted as the solid line 2(a) from their expression D = 0.40 exp (-44,090/RT). Also for comparison, the lowest temperature point of Hoffman and Tumbull3 is plotted. It is apparent that our data diverge appreciably from the high-temperature extrapolation by 373°C. A better straight line fit for the low-temperature portion is obtained by subtracting the extrapolated volume diffusion coefficient from the apparent. or measured coefficient, and plotting the difference, curve (h) of

Jan 1, 1970

By H. J. French

At the request of a committee of the Engineering Division,&apos; National Research Council, a study of the properties of boiler plate at various temperatures up to about 900&apos; F. (482" C.) has been instigated. The following is a report of preliminary tests made on two grades of 1/2-in. plate and includes a description of the apparatus used in the determination of the proportional limit. Detailed reference to- the many published investigations in connection with the properties of steel at various temperatures will be omitted from this report. Suffice to state that results obtained for variation in tensile strength, elongation, and reduction in area with temperature are in substantial agreement with the effects now generally considered to be correct. Comparison of proportional limit values with results obtained by other investigators will be found in the conclusions. Materials Used The steels tested were $1/2-in. (12.7 mm.) open-hearth boiler plate of firebox and marine grades. The specified tensile strength and the analysis for each are shown in Table 1. In the manufacture of this material, a

Jan 1, 1922

By R. L. Templin

IN TREATING a cast metal by any working process such as rolling, drawing or forging, variations in the conditions present in the remelting, casting, chilling and preheating of the initial ingot will certainly have some effect on the physical properties of the final product. In considering the effects of cold working on the physical properties of metals, however, it will be assumed that these factors, being controlled according to best practice, will remain constant and therefore may be neglected. Starting with such a uniform metal ingot, the next operation in the production of wrought metal involves hot working by rolling, forging or extrusion so as to produce a slab, billet or bloom. This working must be sufficient to produce substantial grain refinement and minimize any defects occurring in the initial ingot. Even such a hot-worked product is not suitable as a starting material for determining the effects of cold working because it contains internal strains analogous to those resulting from cold working. It is necessary, therefore, to supplement the hot working with a considerable amount of cold working, followed by a proper annealing in order to obtain a material suitable for use in defining the effects of cold working on the physical properties of a metal. That is, if the effects of cold working are to be evaluated accurately it is necessary to have other effects at least constant if not absent. Such material, unfortunately, cannot always be obtained in commercial practice but the requirements just indicated certainly represent the desired goal; this goal has been attained in the treatment of some metals, one being aluminum.

Jan 1, 1929

For many years the occurrence of gold in the Coeur d&apos;A1ène region had been rumored among the pioneers of the Northwest. It is stated that as early as 1853 gold was discovered in this district by Donelson, of the Stevens expedition, but the hostility of the Indians prevented prospecting. In 1858, when Lieutenant John Mullan surveyed the military road across the Bitter hot mountains, the members of his expedition, most of whom had mined in California, noticed sundry outcrops of good-looking quartz, and some of them actually found gold, as is recorded in a letter that Mullan wrote, from Washington, in 1884. The first successful prospector in the Coeur d&apos; Alène was Tom Irwin, who worked a quartz vein on the Mullan road in the spring of 1879. Two years later he met A. J. Prichard, who was engaged in the lumber business; he told him what he thought of the chances of placer mining in the upper reaches of the Coeur d7AlBne river. This was in 1881. Prichard became keenly interested, and himself found gold on several creeks, one of which is now known by his name, at a place close to the site of the town of Murray.* In 1883 Prichard located a number of claims, and shortly afterward he wrote a letter to the members of a Liberal League to which he belonged, inviting them to "secure the lion&apos;s share" of the mineral wealth he had uncovered. His letters caused a stampede from Montana and Colorado, and from South Dakota also, to the Coeur d&apos;Alène gold belt in the summer of 1883. A town, named Eagle City, was surveyed; in 1884 lots sold at prices ranging from $200 to $2000. The buildings were made of logs and shingles. Shoveling of the snow in&apos; front left s

Jan 1, 1932

By H. J. French

At the request of a committee of the Engineering Division,&apos; National Research Council, a study of the properties of boiler plate at various temperatures up to about 900&apos; F. (482" C.) has been instigated. The following is a report of preliminary tests made on two grades of 1/2-in. plate and includes a description of the apparatus used in the determination of the proportional limit. Detailed reference to- the many published investigations in connection with the properties of steel at various temperatures will be omitted from this report. Suffice to state that results obtained for variation in tensile strength, elongation, and reduction in area with temperature are in substantial agreement with the effects now generally considered to be correct. Comparison of proportional limit values with results obtained by other investigators will be found in the conclusions. Materials Used The steels tested were $1/2-in. (12.7 mm.) open-hearth boiler plate of firebox and marine grades. The specified tensile strength and the analysis for each are shown in Table 1. In the manufacture of this material, a

Jan 1, 1922

By R. P. Fischer

A large production of vanadium during the war helped Germany to meet her critical requirements for the ferroalloy metals. Vanadium was needed not only in the ordinary high-speed too1 steels, but in other as a substitute for chromium, nickel, and molybdenum, which were scarce. Lacking a source of vanadium ore, however, the vanadium was obtained as a by-product of the steel industry—va-nadium-bearing pig iron smelted from iron ores containing about o. I per cellt V was blown in converters to yield vanadium-rich slag, from which vanadium was recovered by chemical treatment. The production capacity obtained was said to be about 6,500,000 lb. of vanadium a Year. Although the general Processes of Preparing vanadium-rich slags as well as the recovery methods described herein are known, some of the details presented may be of interest to both the American steel industry and the vanadium producers. No adequate data on the cost of the vanadium produced in Germany are known, but it seems likely that the cost exceeds the commonly quoted domestic price of about $1.10 per pound of contained VzOa. Information on the German vanadium production was obtained by a team of geologists from the Geological Survey* United States Department of the Interior, during investigations in May and June 1945 of the German utilization of low-grade raw materials. These investigations were sponsored by the Chief of Engineers, War Department. It is a pleasure to acknowledge the aid obtained from Messrs. H. C. Smith and J. D. Dickerson, investigators assigned to the Army Ordnance section of C.I.O.S., and Mr. C. F. Park, Jr., of the Geological Survey team. The data on vanadium recovery from iron ores were obtained from the Kaiser Wilhelm Institut fiir Eisenforschung, the Hermann Goring steel plant at Watenstedt, and from notes made by other investigators at other German steel plants. Preparation of Vanadium-rich Slags Most German iron ores contain only about 0.1 per cent vanadium, or even less, but some of the scandinavian iron ores available to the German iron industry in the past contain a little more than 0.1 per cent. In general German practice of vanadium recovery, nearly all of the vanadium in the ore goes into the pig iron, which is blown in the Thomas converter, yielding a slag containing about I per cent V. This slag is remelted, the vanadium again going with the iron, which is again blown in a converter, yielding a slag that averages about 10 per cent V. This slag is treated at special chemical plants, by the process of a sodadizing roast, water leach, and acid precipitation of vanadium oxide. The Herman Goring steel plant at Watenstedt used the low-grade Salzgitter iron ores, the average composition of which is shown in Table I, column I. The acid and basic iron produced in the blast furnaces contained about 0.3 per cent V. A Thomas

Jan 1, 1948

By R. P. Fischer

A large production of vanadium during the war helped Germany to meet her critical requirements for the ferroalloy metals. Vanadium was needed not only in the ordinary high-speed too1 steels, but in other as a substitute for chromium, nickel, and molybdenum, which were scarce. Lacking a source of vanadium ore, however, the vanadium was obtained as a by-product of the steel industry—va-nadium-bearing pig iron smelted from iron ores containing about o. I per cellt V was blown in converters to yield vanadium-rich slag, from which vanadium was recovered by chemical treatment. The production capacity obtained was said to be about 6,500,000 lb. of vanadium a Year. Although the general Processes of Preparing vanadium-rich slags as well as the recovery methods described herein are known, some of the details presented may be of interest to both the American steel industry and the vanadium producers. No adequate data on the cost of the vanadium produced in Germany are known, but it seems likely that the cost exceeds the commonly quoted domestic price of about $1.10 per pound of contained VzOa. Information on the German vanadium production was obtained by a team of geologists from the Geological Survey* United States Department of the Interior, during investigations in May and June 1945 of the German utilization of low-grade raw materials. These investigations were sponsored by the Chief of Engineers, War Department. It is a pleasure to acknowledge the aid obtained from Messrs. H. C. Smith and J. D. Dickerson, investigators assigned to the Army Ordnance section of C.I.O.S., and Mr. C. F. Park, Jr., of the Geological Survey team. The data on vanadium recovery from iron ores were obtained from the Kaiser Wilhelm Institut fiir Eisenforschung, the Hermann Goring steel plant at Watenstedt, and from notes made by other investigators at other German steel plants. Preparation of Vanadium-rich Slags Most German iron ores contain only about 0.1 per cent vanadium, or even less, but some of the scandinavian iron ores available to the German iron industry in the past contain a little more than 0.1 per cent. In general German practice of vanadium recovery, nearly all of the vanadium in the ore goes into the pig iron, which is blown in the Thomas converter, yielding a slag containing about I per cent V. This slag is remelted, the vanadium again going with the iron, which is again blown in a converter, yielding a slag that averages about 10 per cent V. This slag is treated at special chemical plants, by the process of a sodadizing roast, water leach, and acid precipitation of vanadium oxide. The Herman Goring steel plant at Watenstedt used the low-grade Salzgitter iron ores, the average composition of which is shown in Table I, column I. The acid and basic iron produced in the blast furnaces contained about 0.3 per cent V. A Thomas

Jan 1, 1948