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By H. R. Ogden, A. G. Imgram, D. N. Williams

The effects of composition on the mechanical properties and aging characteristics of several alloys in the Ti-V-Cr system, with and without aluminum modifications, were evaluated. Increasing the chromium, vandium, or aluminum content increased the strength of quenched structures with chromium being the most effective strengthener. Appreciable aging response was obtained with low chromium alloys, but high chromium alloys age softened rather than. hardened. High vanadium contents had a similar effect. Aluminum additions shifted the aging behavior toward that observed in lower chromium alloys, enabling high chromium alloys to be age hardened. DURING the course of titanium alloy development many a and a-ß alloys have been evolved to commercial status. However, only one all-ß alloy has achieved this same stature. This is the Ti-13V-11Cr-3Al alloy. It is characterized by a very sluggish ß-phase decomposition reaction such that very slow cooling rates can retain the 0 phase at room temperature. In addition, very high strength levels can be obtained by long-time aging treatments. Combinations of cold or warm working followed by aging produce even further improvements in strength. This paper describes the results of a research program in which the effects of composition on the mechanical properties and aging characteristics of several alloys in the Ti-V-Cr system, with and without aluminum modifications, were evaluated. EXPERIMENTAL PROCEDURES Electrolytically refined, high-purity titanium was used as the alloy base for these studies. Iodide chromium, electrolytically refined vanadium granules, and high-purity aluminum sheet were used as alloying additions. The compositions of interest were melted as 250-g ingots in a direct current arc melting furnace under a flowing atmosphere of argon. The ingots were hot forged to 3/4-in.-diam bars, vacuum annealed for 6 hr at 1800°F to reduce residual hydrogen content, and then hot swaged to 1/4-in.-diam rods. Fabrication history, and interstitial analyses after fabrication are given in Table I. All specimens to be heat treated were sealed in Vycor capsules under a partial pressure of argon. Samples used to define the ß transus were quenched from temperatures ranging from 1350° to 1100°F after holding at temperature for 15 min. Samples for aging studies were quenched from above the ß transus temperature and then aged for up to 64 hr at 750°F and for 100 hr at 850°, 900°, and 950°F. The effects of straining prior to aging were also investigated. The results of these studies were used to select the heat treatments for the tensile specimen blanks. Heat treatments of the tensile specimens are described in Table 11. Alloys were aged after solution heat treatment or after solution heat treatment and cold swaging to 50 pct reduction in area. Standard 0.125-in.-diam tensile specimens were machined from the heat-treated blanks. All tensile tests were performed in a Baldwin-Southwark uni-

Jan 1, 1963

SEC. 1. The membership of the Institute shall comprise six classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6, Rocky Mountain Members. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members. SEC. 3. Honorary Members: Each candidate for Honorary Membership must be recommended by at least ten Members and must be elected by ballot at a meeting of the Board of Directors by the unanimous vote of the Directors present; provided, however, that the number of Honorary Members shall at no time exceed twenty. Such election shall automatically act as a transfer of such member from any other class of membership to which he may belong. SEC. 4. Senior Members: The Directors may in their discretion place on the Honor Roll of Senior Members and transfer from any other class of membership other than Honorary Membership the name of any Member or Associate who has reached the age of seventy years and who has paid dues for thirty years, and for good reasons in • special cases may vary the age or number of years. SEC. 5. Junior Members: A person to be eligible for election to the class of Junior Member must be qualified through education or experience to hold a subordinate position in engineering, mining, metallurgical, geological or chemical work. He shall be not more than twenty-seven years of age at the time of election. The rights of the present Junior Associates shall continue until the same expire by limitation of time. SEC. 6. Associates: A person eligible for election or transfer into the class of Associate shall be one, who, in the opinion of the Committee on Admissions and the Board of Directors, is suitable for such election or transfer by reason of his interest in or connection with mining, geology, metallurgy, or chemistry. SEC. 7. Rocky Mountain Members: Membership in a special class of life memberships without annual or other dues and without right to receive the printed literature distributed to other members or the right and privilege of wearing the official badge of technical members, is given to all members of the Rocky Mountain Club at the time of consolidation. These special Rocky Mountain memberships shall be claimable by any member of the Rocky Mountain Club, not already a member of the Institute,

Jan 1, 1929

By Richard M. Foose

Five miles southwest of Mt. Holly Springs, Cumberland County, Pennsylvania, the Philadelphia Clay Co. has been mining and milling a white clay since 1896; for use in white cement, as a filler in rubber, pigment and paper, in the manufacture of insecticides, and for other minor purposes. Until late in 1942, when the mine was abandoned because of labor shortage, combined underground mining and surface stripping produced approximately 30,000 tons of clay a year, of which 10,000 tons were refined in the mill. Geology Lower Cambrian Antietam quartzite and the Rilontalto quartzite, stratigraphi-cally older, trend N.55°E. and make a sharp 1600-ft. anticlinal ridge of the South Mountains. The Tomstown dolomite overlies the Antietam quartzite on the southeast flank of the anticline, which is displaced near its crest by a steeply dipping oblique fault. Erosion of the less resistant Tomstown formation has resulted in a narrow valley at an elevation of 700 ft. Directly on top of the Antietam quartzite and at the base of the Tomstown formation is a zone of sandy white clay, lenticular along the strike of the formations, ranging in thickness from 10 to 300 ft. within a mile. All of the formations dip steeply to the southeast, from 65" to vertical. The clay crops out at an elevation of about 1000 feet. Origin and Character The uppermost part of the Antietam formation is sericitic and schistose at many places, and at all these places weathering is in an advanced stage. The clay is the residual product of weathering of this sericitic quartzite or sandy schist. The crude clay has the physical aspect of a sandy kaolin, but there Are large areas in the clay formation that are low in free silica, and commonly the 30 ft. adjacent to the Antietam quartzite is notably free of silica. The overlying Tomstown dolomite has been weathered almost completely to a mixed yellow and brown clay, which carries a zone of nodular and chunky limonite and manganese ore, 4 to 12 ft. thick, about loo ft. from the contact with the white clay. In mining, this zone is an important "marker," indicating where the white clay may be expected in an advancing tunnel. The contact of the white clay formation with the yellow and brown clay of the Tomstown formation is relatively sharp, although the line of contact is irregular and therefore responsible for the lenticular character of the white clay formation. Following is an analysis of the refined clay containing less than one per cent of moisture when dried at 212°F.: SiO2, 67.05 per cent; Al2O3, 22.27; Fe2O3, 0.40; CaO, 0.00; TiO2, 1.05; MgO, 0.52; Na20, 0.04; K2O, 0.88; ignition loss, 7.65; total, 99.86.

Jan 1, 1948

By John M. Sharp

John M. Sharp, Jr. (Assistant Professor of Geology, University of Missouri, Columbia, Mo.)-Geothermal gradient and surface temperature data anomalies are potentially useful tools in mineral exploration, These data, however, may reflect a number of geologic and hydrologic processes as well as the thermophysical properties of the geologic materials. The author presents a relatively simple model which may be of value in mineral exploration. The lack of consideration of other processes, however, limits its usefulness. For instance, because of erosion or sediment deposition over geologic time the land surface must be considered a moving boundary in such a model. Evaluation of this effect coupled with annual surface temperature and thermal conductivity variations can result in temperature profiles such as shown in [Figs. 4 to 7]. These effects and others, such as ground-water movement," must be considered and filtered from the data before proper interpretation is possible. Another assumption which should have been discussed is, why were the observed mean surface temperatures not used for extrapolation of the gradients in [Figs. 4, 6, and 7?] Conductive heat transport responds to the actual boundary (land surface) temperature, not to theoretical temperatures in the absence of perturbations. Benfield presents a theoretical model for calculating perturbations in the geothermal gradient for erosion and sedimentation. The temperature (T) at any time (t) and any depth below the surface (x) is given by [ ] where T is the mean surface temperature, G, the geothermal gradient, v, the rate of erosion (or sedimentation),[ ], the long-term rate of change of T0, and k is the thermal diffusivity of the rock. Using the author's values and a rate of erosion of 1.54 cm per yr for a period of 10,000 yr, a thermal profile as shown in [Fig. 10] will be generated. A thermal diffusivity of 0.0164 sq cm per sec was used, corresponding to a thermal conductivity of 0.0082 cal per cm per sec per C. In [Fig. 11], a sediment deposition rate of 3.0 cm per yr for a period of 1000 yr was used to generate the subsurface temperature profile. A surface temperature of 24.3°C was used, as specified in [Fig. 9, 7], was set equal to zero for both cases. Superposition on the generated profiles in [Figs. 10 and 11] of the annual surface temperature variation perturbation (which may be calculated in a number of ways) will yield profiles similar to those in [Figs. 4 and 7]. Similar profiles can also be produced by regional ground-water flow. Models like the author's can be of value in mineral exploration. Other processes, however, which affect surface temperatures and gradients must first be considered, calculated, and filtered from the data if anything but the crudest qualitative interpretation is to be made. Robert C. Edmiston (Author's reply)-Professor Sharp has raised three objections to my interpretation of the subsurface temperature data I collected at Silver Bell. These are: 1) No correction was made for erosion or sedimentation,

Jan 1, 1977

By H. R. Hendricks

THE ore of the Iron King Mine, being very hard and having a very fine crystalline structure, presents many problems in milling that are not present in ordinary lead-zinc ores. This very fine crystallization causes much interlocking of minerals and is most prevalent between the gold and pyrite and the sphalerite and pyrite. The recovery of gold is extremely important in the economic value of the ore and therefore constitutes a large part of the metallurgical problem to be solved. All of the gold is free but it has not been observed in any of the mill products except under very high magnification. Some of the gold is tarnished, and this condition also makes recovery difficult. The gold values have been determined to be highest in association with chalchopyrite and arsenopyrite. The silver occurs mostly in association with galena and tennantite. A small amount of native silver has also been observed occasionally. The galena, being softer than the other minerals, frees much better in grinding. Some oxidation of galena is present in the ore, as the nonsulphide lead content amounts to approximately 10 pct of the total lead. Some oxidation of sphalerite is also present in the ore. Microscopic examination of the zinc concentrate shows many grains in the minus 325-mesh to be half pyrite, together with the fact that some of the zinc is marmatite, makes production of a high-grade zinc concentrate very difficult unless recovery is sacrificed. In the grinding, it has been determined that the flotation feed must be maintained at 85 pct minus 200-mesh to free the minerals sufficiently to make the best economic recoveries. Table I illustrates the effect of fine grinding. It shows that the bulk of the recovered minerals is in the minus 325-mesh size and is the part of the minerals that is more readily freed. The pyrite concentrate is not given in the table because it contains practically no minus 325-mesh. DEVELOPMENT OF PRESENT FLOWSHEET AND MILLING PRACTICE The first milling operation started in 1938, with a mill capacity of 140 tons daily, producing a bulk gold-silver-lead concentrate. After several stages of expansion and changes of the mill flowsheet, the mill is currently treating 380 tons of ore daily and three separate concentrates are produced. In order of their importance and value, these are: (1) lead concentrate, (2) zinc concentrate and (3) pyrite concentrate. The present average grade of mill heads is: gold 0.11 oz, silver 4.00 oz, lead 2.50 pct, zinc 7.60 pct, copper 0.22 pct, iron 22 pet and 30 pct insolubles. Specific gravity of the ore is 3.8. During the period when bulk flotation was practiced, the flowsheet was very simple. The ore was ground fine enough to liberate as much gold, silver and lead as possible. Necessary collectors and frothers were added in sufficient quantity

Jan 1, 1947

By Richard M. Foose

Five miles southwest of Mt. Holly Springs, Cumberland County, Pennsylvania, the Philadelphia Clay Co. has been mining and milling a white clay since 1896; for use in white cement, as a filler in rubber, pigment and paper, in the manufacture of insecticides, and for other minor purposes. Until late in 1942, when the mine was abandoned because of labor shortage, combined underground mining and surface stripping produced approximately 30,000 tons of clay a year, of which 10,000 tons were refined in the mill. Geology Lower Cambrian Antietam quartzite and the Rilontalto quartzite, stratigraphi-cally older, trend N.55°E. and make a sharp 1600-ft. anticlinal ridge of the South Mountains. The Tomstown dolomite overlies the Antietam quartzite on the southeast flank of the anticline, which is displaced near its crest by a steeply dipping oblique fault. Erosion of the less resistant Tomstown formation has resulted in a narrow valley at an elevation of 700 ft. Directly on top of the Antietam quartzite and at the base of the Tomstown formation is a zone of sandy white clay, lenticular along the strike of the formations, ranging in thickness from 10 to 300 ft. within a mile. All of the formations dip steeply to the southeast, from 65" to vertical. The clay crops out at an elevation of about 1000 feet. Origin and Character The uppermost part of the Antietam formation is sericitic and schistose at many places, and at all these places weathering is in an advanced stage. The clay is the residual product of weathering of this sericitic quartzite or sandy schist. The crude clay has the physical aspect of a sandy kaolin, but there Are large areas in the clay formation that are low in free silica, and commonly the 30 ft. adjacent to the Antietam quartzite is notably free of silica. The overlying Tomstown dolomite has been weathered almost completely to a mixed yellow and brown clay, which carries a zone of nodular and chunky limonite and manganese ore, 4 to 12 ft. thick, about loo ft. from the contact with the white clay. In mining, this zone is an important "marker," indicating where the white clay may be expected in an advancing tunnel. The contact of the white clay formation with the yellow and brown clay of the Tomstown formation is relatively sharp, although the line of contact is irregular and therefore responsible for the lenticular character of the white clay formation. Following is an analysis of the refined clay containing less than one per cent of moisture when dried at 212°F.: SiO2, 67.05 per cent; Al2O3, 22.27; Fe2O3, 0.40; CaO, 0.00; TiO2, 1.05; MgO, 0.52; Na20, 0.04; K2O, 0.88; ignition loss, 7.65; total, 99.86.

Jan 1, 1948

By H. C. Chao, Y. E. Smith, L. H. Van Vlack

ThE phase relationships for the MnO-MnS system have been investigated only in the eutectic region. wentrupl reported a eutectic at 1280°C (2345°F) with approximately 50 wt pct of each component, as based on the earlier work of Andrew, Maddocks, and Fowler.2 More recently silverman3 corrected these figures to 2275° ±10°F (1246°C) with 63 wt pct MnS and 37 pct MnO. Neither Wentrup nor Silverman investigated the solid-solution limits in this system. However, Wentrup did suggest with his phase diagram sketch that the maximum solubility of MnS in MnO is 10 wt pct, and the solubility of MnO in MnS is nearer 20 wt pct, Fig. 1. These figures have been utilized in subsequent publications without further verification.4 There had been evidence found in this laboratory that the above solid-solution figures were high. An investigation was therefore conducted using the following procedure. Samples containing MnO and MnS were contained in platinum foil, heated just above the eutectic temperature in a purified nitrogen at- mosphere, and quenched into distilled water. The MnO had been prepared by calcining reagent grade MnCO3 in nitrogen at 1400°C. Only MnO was detected in subsequent X-ray diffraction analyses. The MnS had been prepared by sulfur deoxidation of reagent grade MnSO4 according to the reaction: MnSO4 + S2 ? MnS + 2SO2 The details of the sulfide preparation procedure, which utilized atmospheric sulfur pressures at 950°C, are discussed elsewhere.5 The sulfur content of the sulfide was determined to be 36.8 * 0.2 pct, which matches the stoichiometric value of 36.9 pct. No evidence of either MnO or MnSO4 was detected microscopically or by X-ray diffraction. The single-phase combinations of MnO and MnS at the eutectic temperature indicate the limit of solid solution as shown in Fig. 2(a) and (c), and the revised phase diagram is shown in Fig. 2(d). The melting temperature for MnO is that provided by Glasser.6 The eutectic temperature of 1232° ± 5°C and eutectic composition of 64 wt pct MnS are in close agreement with Silverman's correction of Wentrup's work. The maximum solubility of MnO in MnS was determined to be 1.7 ± 0.2 wt pct. The maximum solubility of MnS in MnO was determined to be 1.8 ± 0.2 wt pct. These figures represent the lower limit for the presence of liquid at 1260°C and are significantly lower than the earlier estimated solid-solution figures. The authors wish to acknowledge the support of U.S. Steel's Edgar C. Bain Laboratory for Fundamental Research. The comments and critical suggestions of Drs. A. S. Keh, R. Rickett, and R. B. Snow are appreciated.

Jan 1, 1963

By Arch J. Alexander

This paper is a resume of a study undertaken by the West Virginia Department of Mines. The underlying and direct causes of accidents are determined in each occupational group. Then from this study, accident prevention courses, visual and written, are to be taken to the various working groups in the mines. THE causes of accidents in West Virginia mines follow the main pattern of coal industry accidents in the United States—falls of roof, ribs and face, 56 pct; from haulage, 25 to 30 pet; blasting, 3 pet; electrocutions, 3 pct; explosions, 2 pct; and other causes, about 10 pct. To arrive at some satisfactory conclusions regarding causes and prevention of mine accidents, the Department of Mines has made a study of all mine accidents, from 1945 to 1948, inclusive. During the last two years of this period, we did not have a major explosion, one that took the lives of as many as five men. The direct cause of these accidents is apparent in the reports but we who are making a close study into their frequency think that the virus lies much deeper, and we want to suggest an underlying cause. The rapid growth of the coal industry in West Virginia, the largest producer of bituminous coal, has resulted in a demand for manpower which probably has never been equaled in mining history. At the turn of the century, West Virginia had 24,635 men employed in and about her mines, and they produced 21,153,341 tons of coal a year. In 1948, there were 125,669 men employed, and coal production for the year was 168,589,033 tons, an average increase of 35 pct for each year since 1900. Over 100,000,000 tons of this increase were mined in the southern counties of the state. A safety analyst might read into the history of this development an underlying cause for accident occurrence. He might say that in such a vast, rapid development the available supply of trained miners became exhausted and that young, inexperienced men were employed in the mines by the thousands. Being unacquainted with the hazards of mining, it would be only natural for these young men to be injured or killed in too great a number. This assumption would not be borne out by the records. Men were not injured or killed in disproportionate numbers during their first years in a mine. The only reason we can give is that, during these years, they possessed an attribute of safety—CAUTION—to a much greater degree than in the years following. The coal companies in West Virginia that have been operating over a number of years have a nucleus of employees who have been with them ten, twenty, thirty, and forty years; many of them having gained all of their mining experience with one company. Their habits of work have been

Jan 1, 1951

By Arch J. Alexander

This paper is a resume of a study undertaken by the West Virginia Department of Mines. The underlying and direct causes of accidents are determined in each occupational group. Then from this study, accident prevention courses, visual and written, are to be taken to the various working groups in the mines. THE causes of accidents in West Virginia mines follow the main pattern of coal industry accidents in the United States—falls of roof, ribs and face, 56 pct; from haulage, 25 to 30 pet; blasting, 3 pet; electrocutions, 3 pct; explosions, 2 pct; and other causes, about 10 pct. To arrive at some satisfactory conclusions regarding causes and prevention of mine accidents, the Department of Mines has made a study of all mine accidents, from 1945 to 1948, inclusive. During the last two years of this period, we did not have a major explosion, one that took the lives of as many as five men. The direct cause of these accidents is apparent in the reports but we who are making a close study into their frequency think that the virus lies much deeper, and we want to suggest an underlying cause. The rapid growth of the coal industry in West Virginia, the largest producer of bituminous coal, has resulted in a demand for manpower which probably has never been equaled in mining history. At the turn of the century, West Virginia had 24,635 men employed in and about her mines, and they produced 21,153,341 tons of coal a year. In 1948, there were 125,669 men employed, and coal production for the year was 168,589,033 tons, an average increase of 35 pct for each year since 1900. Over 100,000,000 tons of this increase were mined in the southern counties of the state. A safety analyst might read into the history of this development an underlying cause for accident occurrence. He might say that in such a vast, rapid development the available supply of trained miners became exhausted and that young, inexperienced men were employed in the mines by the thousands. Being unacquainted with the hazards of mining, it would be only natural for these young men to be injured or killed in too great a number. This assumption would not be borne out by the records. Men were not injured or killed in disproportionate numbers during their first years in a mine. The only reason we can give is that, during these years, they possessed an attribute of safety—CAUTION—to a much greater degree than in the years following. The coal companies in West Virginia that have been operating over a number of years have a nucleus of employees who have been with them ten, twenty, thirty, and forty years; many of them having gained all of their mining experience with one company. Their habits of work have been

Jan 1, 1951

By S. C. Sircar, B. K. Dhindaw

KINETICS and mechanism of sulfation reactions have been studied extensively. Qualitative and quantitative data are reported for the kinetics and mechanism of sulfation reaction of copper oxide pellets;''2 yet it remains a controversial Subject. The mechanism and kinetics of the sulfation of zinc oxide powder (B.D.H. analar quality) were studied by gravimetric technique. A spring of high-carbon steel wire with accuracy well within 0.2 mg was used for measuring weight change. The sample was taken in a Pyrex glass bucket, hanging freely inside a Pyrex glass tube reactor, with a gold wire attached to the spring, the reactor being surrounded by a movable furnace (double wound type) with a temperature control within *5"C. Flow of oxygen, 60 cu cm per min, and sulfur dioxide, 45 cu cm per min, were measured through calibrated flowmeters and the mixture dried over PZ05 before entering the reactor. The experimental results are presented in Figs. 1 and 2. The plot of weight change of zinc oxide, giving the amount of zinc sulfate formed, was found to be linear over the temperature range of 500" to 700° C and up to a conversion of approximately 60 pct, as beyond it they divert from linearity.' The rate of sulfation was found to be affected by total flow rate of gases at a fixed ratio of SO2/O2, up to 60 cu cm per min, and was found to be linearly dependent on quantity of total powdered sample taken. The plot of rate of sulfation of zinc oxide, 70 mg, with varying amounts of vanadium pentoxide, at a constant ratio of gases as mentioned above, and at a constant temperature of 625"C, was also found to be linear as seen in Fig. 2. Extrapolation to zero V2O5 addition gives the same rate of sulfation, as in case of pure zinc oxide, 70 mg. Vz05 was prepared by heating ammonium vanadate at 600°C for 15 min in a muffle furnace. The available literature points out that the theory of sulfation that has received the maximum support postulates the following mechanism for sulfation of ZnS: 2ZnS + 30, = 2Zn0 + 2SOZ; the ZnO formed acts as a catalyst for the reaction, 2 S02 + O2 = 2S03. This SO3 reacts with ZnO to give zinc sulfate. It is suggested here that the above widely supported mechanism is operative in the sulfation reaction and that the rate-controlling step in the sulfation reaction of ZnO is the formation of SO3 from SO, and 0,. The authors are carrying on further work in this line, and the details will be published later. The authors wish to acknowledge the facilities provided and the help extended by Prof. P. R. Dhar, Head, Department of Metallurgical Engineering, and the permission granted to publish this note by the Director, I. I. T., Kharagpur.

Jan 1, 1969

By K. L. Moazed, G. M. Pound

An investigation was made of the deposition of silver from a thermal beam onto tungsten field-emitter tips at 300°K. "Island"-type nuclei were observed to form and grow. The nucleation of silver crystals occurs preferentially on non-close -packed planes of a tungsten tip at a critical volume free-energy change of about —2900 cal per cc. The adatom population which is critical for appreciable nucleation rate of silver crystals is about 0.2 of a monolayer and is essentially independent of beam flux, time, and source temperature. This result is strong evidence that a metastable equilibrium exists between adatoms and critical nuclei, as assumed in the present theory. SOME of the more significant studies of nucleation in deposition of metals from vapor beams have been conducted by measuring the thermal beam flux which is critical for appreciable rate of nucleation on a substrate surface held at a given temperature.'2 The observed critical supersaturations may be described in terms of Eq. [7] which was derived3'3a on the model of an adsorption, surface migration, and statistical fluctuation mechanism. However there usually made with a low-power optical microscope, a fairly insensitive method of detection. The object of the present study was to overcome some of these difficulties by measuring the critical supersaturation for condensation of a thermal beam of silver onto a tungsten field-emitter tip. Such a tip may be cleaned by electrically heating it to a high temperature in situ, and the high vacuum obtainable in a field-emission tube (10-10 torr) precludes adsorption of residual gases for convenient periods of time. Furthermore, the degree of cleanliness, the orientation, and the state of imperfection of the tip may be ascertained from the field-emission pattern. Detailed explanations of theoretical considerations and experimental procedures relating to the field-emission microscope may be found in a number of excellent review articles12'13 and thus only a brief description will be given here. The electronic work function of a metal is defined as the energy that an electron needs to escape from the potential field of the solid. By applying a large field between the surface of the solid and a suitable collector, it is possible to free the electrons by the tunnel effect. Fields of approximately 30 million v per cm are needed to produce this effect, and such fields are obtained in practice by using microscopic surfaces of high curvature (tips). Because the work function of a metal is a function of surface orientation, the emission from the various planes is different, and thus it is possible to obtain a representation of the surface in the emission microscope. In general, the work function is higher for the more densely packed planes. Fig. 1 shows a pattern for "clean" tungsten in which the central dark region represents the (110)

Jan 1, 1964

By P. W. Barton, A. A. Johnson, E. J. Hughes

THE only systematic work on the effect of carbon on the recovery and recrystallization kinetics of iron so far reported in the literature is that of Venturello et al.1 These workers found that doping high-purity iron so that it contained up to 86 ppm C caused a marked retardation of recovery but had little or no effect on the recrystallization kinetics. Such evidence for an effect as was obtained was inconclusive. In the course of a study of electron-beam zone-refined iron the authors have recently examined the effect of added carbon on the recrystallization kinetics of this material. The amount of carbon added was about 50 pct more than was used by Venturello et 01. and definite evidence was obtained that carbon at this level retards recrystallization. The starting material was taken from a batch of 0.2-in.-diameter Johnson-Matthey spectroscopically pure iron rods which had been further purified by being given three passes at 4 in. hr-1 in a standard MRC electron-beam zone-refining unit. The purity of this material. which was used in two other investigations of the properties of high-purity iron,2,3 was established by an extensive series of analyses. Four laboratories, the National Research Corp., Newton, Mass., the Naval Research Laboratory, Washington, D.C.. the Battelle Memorial Institute, Columbus, Ohio, and the National Physical Laboratory. Teddington. Middlesex, England. carried out analyses for carbon. oxygen. and nitrogen. and in addition a complete mass-spectrograph analysis was carried out at Battelle. In all, twelve analyses were carried out for carbon, seventeen for oxygen and twelve for nitrogen. The amounts of these elements found to be present were 10 * 7, 8 i 5, and 0.9 i 0.1 ppm, respectively. The limits given are rms deviations. Two results, one of 46 ppm of oxygen and another of 31 ppm of nitrogen, were rejected as anomalous. The mass-spectrograph analysis revealed the major impurity to be 25 ppm of tungsten. All of the other elements detected were present in amounts less than 0.5 ppm. Some of the rods were doped with carbon by being immersed in a suspension of carbon in oil, heated in a vacuum at 400°C, and then zone-leveled to make the distribution of carbon uniform. Carbon analyses carried out on three of the doped rods gave a mean value of 130 ± 45 ppm. Some of the doped and undoped rods were deformed 58 pct by swaging and cut into specimens 1/2 in. in length. Isothermal recrystallization experiments were then carried out on them at 575", 600°, 615", 630°, and 650°C, the volume fraction of each specimen recrystallized being measured by a point-counting method described by Hilliard and Cahn.4 The results for the two types of specimens are shown separately in Figs. 1 and 2. In Fig. 3 the pairs of recrystallization curves for each temper-

Jan 1, 1965

By R. F. Ashton, D. S. Thompson

In reporting results of precipitation hardening experiments, it is customary to include such conditions as solution heat-treatment temperature, specimen size, and quench medium as well as the aging time and temperature. One portion of thermal history that is often overlooked is the effect of the heating rate employed to achieve the aging temperature. It is the intent of this note to demonstrate the importance of the rate of heating to aging temperatures. This work was carried out on the aluminum alloy 7075 aged at 162oC, a temperature commonly used to obtain stress corrosion resistant tempers. A 2 in. thick plate of 7075 was quenched into 24°C water after solution heat-treatment for 2 hr at 470°C. Approximately 13 in. around the periphery of the plate was discarded to minimize quench rate variations, and the remainder was divided into 0.5 by 1.8 by 2.0 in. blocks which were held at room temperature, 24oC, for 4 days. This aging, or incubation period, at room temperature allowed a copious supply of GP-zones to form. Blocks were then heated at various rates to 162oC using the practices shown in Table I. Both single- and two-step aging practices were employed for each heating rate. The single step consisted of heating directly to temperature at the indicated rate while the two-stage practice included an interruption of heating for 7 hr at 107°C. In the case of the two-stage 100°C per min heating rate experiment, the specimens were returned to room temperature after 7 hr at 107°C where they were held for 16 hr be-fore finally heating at this rate to 162°C. This devia-tion in practice is not considered to be significant. Blocks were removed after various times at 162oC, and aging curves were determined from duplicate R. F. ASHTON and D. S. THOMPSON,Member AIME, are Senior Scientists, Metallurgical Research Division, Reynolds Metals Company, Richmond. Va. Manuscript submitted December 2. 1968. IMD Table I. Aging Practices Two-step Single-Step Heating Rate* Aging Aging Heating Method oC per Min A B Programmed Air Oven 0.23 * 0.01 C D Programmed Air Oven 0.93 ? 0.03 E F Air Oven at Temp -10 G H Oil Bath at Temp ˜100 *Heating rate was measured with a thermocouple at the center of a specimen. An average value between the starting temperature and 3°C below the aging temperature is reported for practices E-H. PRACTICES 70 — A B C E and G 50 - 2 4 6 810 20 40 60 HRS.AT 162°C Fig. 1—The influence of processing variables on 7075 aging curves. Fig. 2—7075 aged according to practice H (single-step aged, fast heating rate) for 3 hr. Magnification 100,000 times.

Jan 1, 1970

By Nicholas J. Grant, H. C. Chang

EMPHASIS on the importance of grain boundary sliding as a mode of deformation at elevated temperatures has been presented elsewhere.' The extent to which boundary sliding occurs under certain creep conditions has been determined for high purity aluminum2,3 and aluminum alloys.' In general, boundary deformation extends quite far into the adjoining grains, resulting in a rather wide band of deformation along the grain boundaries. This has led some investigators to doubt that grain boundary sliding consists of shearing along the boundary surface; it has been contended instead that boundary sliding is a result of concentrated slip in the neighborhood of the deformed grain boundaries."' The purpose of this note is to present evidence that grain boundary sliding takes place by a bulk shear process. gh purity polycrystalline aluminum, wherever and whenever there is grain boundary sliding, boundary migration and concentrated deformation along both sides of the deformed boundary are associated with it. Therefore, it has been rather difficult to obtain unambiguous evidence of boundary sliding. On the other hand, it would be expected in certain alloys of aluminum, when tested under particular conditions. that the severity of the interfering effects of boundary migration and concentrated deformation along the deformed boundary might be reduced. Current research in this laboratory' shows that a 20 pct Zn-A1 solid solution alloy fractures in an intercrystalline manner during creep at 500°F with a small total elongation of not more than about 14 pct, and that it does so with extremely limited grain boundary migration. Accordingly, this alloy was chosen for the present study. The experimental procedure was similar to that used in previous work and has been presented elsewhere.' Two parallel flat surfaces were milled from a round specimen. The gage portion of the specimen was 1 in. x .09 in. x .17 in. The specimens, which were annealed at 1030°F for 24 hr, showed two to four grains across the width of the test bar. The specimens were subjected to creep at 500°F at stresses of 2000 to 5000 psi. The rupture times were from 10 sec to 3 hr. Appreciable boundary sliding occurred in all the tests. A typical example of boundary sliding is shown in Fig. 1. (The tension axis is vertical in the micrographs.) Sliding has taken place along the boundary between grains A and B unaccompanied by important boundary migration. The sharpness of the offset at the triple point can be clearly seen in grain C. As a result of sliding along the boundary between grains A and B, a new boundary surface between grains A and C was created. The offset at the triple point is about 0.07 mm. This boundary sliding is accompanied by the formation of rather sharp kinking bands and, of course, slip on several slip systems in grain C. This type of deformation has been referred to as fold formation' in previous work with high purity aluminum.

Jan 1, 1957

By H. H. Kellogg

Available high-fernperatzwe equilibrium measurements and other thermochernical data have been critically reciewed for sulfation reactions of the type: Recommended values for log K and ?Fo as junctions of temperature are given for thirty-six suck reactions involving twenty-six different metals. Methods of calculation and choice between conflict-ing data are discussed. SELECTIVE sulfation now enjoys a considerable renaissance as a metallurgical unit process due, in large part, to the available of the fluid-bed re- actor—a device capable of the close control of temperature and gas composition necessary for a successful sulfation process. An additional need, however, if sulfation chemistry is to be approached in a scientific manner, is a reliable body of data on the equilibrium and kinetics of sulfation reactions in simple and complex systems. This paper offers a critical review and compilation of equilibrium data on pure sulfates (simple systems). The last such review, by K. K. Kelley in 1935:30 has proven itself most useful, but the existence of many new data makes necessary a re-evaluation of the available information. METHODS OF CALCULATION For a simple sulfation reaction such as MS04(c) = MO(c) + SO3 [1] there are two approaches one may take toward establishing the value of ?Fo or K as a function of

Jan 1, 1964

By Howard Scott, Henry S. Rawdon

The method of demonstrating the structure existing in a metal or alloy at high temperatures, by etching a polished sample after it has been heated to the desired temperature, is quite familiar to metallog-raphists. The usual procedure1 2 is to heat the specimen, previously polished for microscopic examination, to the desired temperature, in a neutral atmosphere (hydrogen or nitrogen), then admit the etching gas (chlorine, hydrochloric acid or similar gas) for a few seconds, and finally, after flushing out the etching gas with the neutral one, cool the specimen in the neutral atmosphere. The pattern produced by etching at a definite temperature is usually taken as a record of the microstructure prevailing at that temperature. It has frequently been pointed out that changes in composition of the surface metal occur during the preliminary heating in the neutral atmosphere, so that the appearance produced by the etching at high temperature may not exactly represent the condition of the interior of the specimen. To overcome this uncertainty, the heating has sometimes been done in vacuo,3 the etching gas being admitted when the desired temperature was reached, then pumped out and the specimen cooled in vacuo. The studies of Rosenhain, Humfrey, and other workers 4, 5, 6, 7, 8 dem-

Jan 1, 1922

By Howard Scott, Henry S. Rawdon

The method of demonstrating the structure existing in a metal or alloy at high temperatures, by etching a polished sample after it has been heated to the desired temperature, is quite familiar to metallog-raphists. The usual procedure1 2 is to heat the specimen, previously polished for microscopic examination, to the desired temperature, in a neutral atmosphere (hydrogen or nitrogen), then admit the etching gas (chlorine, hydrochloric acid or similar gas) for a few seconds, and finally, after flushing out the etching gas with the neutral one, cool the specimen in the neutral atmosphere. The pattern produced by etching at a definite temperature is usually taken as a record of the microstructure prevailing at that temperature. It has frequently been pointed out that changes in composition of the surface metal occur during the preliminary heating in the neutral atmosphere, so that the appearance produced by the etching at high temperature may not exactly represent the condition of the interior of the specimen. To overcome this uncertainty, the heating has sometimes been done in vacuo,3 the etching gas being admitted when the desired temperature was reached, then pumped out and the specimen cooled in vacuo. The studies of Rosenhain, Humfrey, and other workers 4, 5, 6, 7, 8 dem-

Jan 1, 1922

By Charles M. Brown, Russell Franks, W. O. Binder

Occasionally in the application of the austenitic chromium-nickel steels to corrosive conditions, failures have occurred by cracking without serious general over-all attack of the metal. As pointed out by Foyt and Scheil(1),2 and by Scheil, et al.(2) as well as by Hodge and Miller(3), the stress-corrosion failures that have occurred have been limited in number, and have taken place only when the steels were exposed to certain corrodents. These investigators have stated that while stress- corrosion cracking can be intergranular in nature and originate at the grain boundaries of the austenitic chromium-nickel steels, it can also take place in trans- granular fashion. They have shown that the cracking may be either initiated at the grain boundaries and may propagate along grain boundaries for some distance and then suddenly extend across grains, or it may begin in a transgranular fashion and suddenly proceed along grain boundaries until the cracking stops. Their data further show that when austenitic stainless steel is subject to intergranular attack, stress will concentrate and cause cracking in service. These investigators have studied the effect of the metals titanium and columbium which are added to the steels to impart immunity to intergranular attack, and molybdenum which is added to improve resistance to general corrosion.

Jan 1, 1945

By D. J. McAdam

Results of investigation of corrosion-fatigue of metals at the U. S. Naval Engineering Experiment Station have been presented by the author in four papers.1, 2, 3, 4 In those papers references were given to the work of Haigh in 1917.5 The investigation at Annapolis included a variety of ferrous and non-ferrous alloys. The experiments showed that even slight corrosion simultaneous with fatigue may cause failure at stresses far below the ordinary endurance limit. The experiments also showed that, for most metals, severe stressless corrosion prior to fatigue is much less damaging than even slight corrosion simultaneous with fatigue. The term "corrosion-fatigue" was restricted to mean the simultaneous action of corrosion and fatigue. The combined effect of corrosion followed by fatigue was called "prior-corrosion fatigue." A stress-cycle graph representing corrosion-fatigue is a curve approaching a horizontal asymptote, the ordinate of which may be called a "corrosion-fatigue limit." To avoid confusion in later discussion, the term "endurance limit" will be restricted to mean the fatigue limit obtained by tests in air with specimens as free as possible from stress concentration and from corrosion. The cndursnce limit as thus obtained presumably represents an inherent property of the metal.

Jan 1, 1929

By D. J. McAdam

Results of investigation of corrosion-fatigue of metals at the U. S. Naval Engineering Experiment Station have been presented by the author in four papers.1, 2, 3, 4 In those papers references were given to the work of Haigh in 1917.5 The investigation at Annapolis included a variety of ferrous and non-ferrous alloys. The experiments showed that even slight corrosion simultaneous with fatigue may cause failure at stresses far below the ordinary endurance limit. The experiments also showed that, for most metals, severe stressless corrosion prior to fatigue is much less damaging than even slight corrosion simultaneous with fatigue. The term "corrosion-fatigue" was restricted to mean the simultaneous action of corrosion and fatigue. The combined effect of corrosion followed by fatigue was called "prior-corrosion fatigue." A stress-cycle graph representing corrosion-fatigue is a curve approaching a horizontal asymptote, the ordinate of which may be called a "corrosion-fatigue limit." To avoid confusion in later discussion, the term "endurance limit" will be restricted to mean the fatigue limit obtained by tests in air with specimens as free as possible from stress concentration and from corrosion. The cndursnce limit as thus obtained presumably represents an inherent property of the metal.

Jan 1, 1929