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THE Annual Fall Meeting held in Chicago in conjunction with the celebration of a Centennial of Engineering brought forth a round of field trips and symposiums which did much to add to the store of information of the 240 who registered for the gathering. Instead of a scattered program, technical papers were grouped together in organized symposiums, where the particular importance of each report was enhanced by presentation in context. Despite the heavy accent on technical papers and informative field trips, those attending the meeting had ample time to enjoy the benefits of a visit to Chicago. The AIME dinner dance was held at the Palmer House, in the Red Lacquer Room. The Chicago Section played host Friday evening at dinner. The MBD held four sessions at the meeting headquarters, the Palmer House, September 4 and 5. Featuring the meetings was a review of taconite concentration and new theories on comminution. The first session opened with a paper on the Structural Features Which Effect the Concentration of Iron Formations, presented by F. J. Tolonen. The paper was centered upon the various members of the low grade iron formations of the separate Michigan districts. The study correlated macrostructure, microstructure, and concentration tests. [ ] Beneficiation Characteristics of Michigan Low Grade Iron Ores, presented by F. X. Tartaron, cochairman of the session, reviewed the work of his laboratory on the beneficiation of low grade ore taken from various strata of a deep shaft on the Marquette Range. The paper included data on flotation, gravity separation, magnetic separation, and combinations of these processes. The economics of low grade ore treatment generated great interest. Ty. Maki offered a compilation and correlation of field results with magnetic separators in ferrosilicon and magnetite medium recovery circuits. Following the morning session, 130 persons attended a luncheon, followed by a brief business meeting. Later, a film illustrating the grinding, separation, and pelletizing steps investigated by the Mines Experiment Bureau, was presented by H. H. Wade. T. E. Ban, and L. J. Erck gave a report on pelletizing which evoked much discussion. R. A. Limons presented a paper on the Mineralogy of Blast Furnace Sinter, for its author, H. M. Kraner. Friday sessions featured a new hypothesis for high speed drill rod milling and a new technical approach to comminution. Jack Myers commented that Consolidated's large rod mill was a hammer mill turned inside out. Steve Erickson described the use of Cyclones for Heavy Media Concentration of Iron Ore Fines. Bob Meaders gave a Progress Report on the Aerofall Mill. Shiou-Chuan Sun described an improved high frequency analyzer for studying the conductivity of suspensions of various minerals. L. A. Roe discussed a magnetic reflux condensor which enabled him to determine the degree of liberation of magnetic iron ores. Roy A. Johnson described a function of the hydroscilator in which the fan rake was eliminated in favor of a conical bottom. The Industrial Minerals Division sessions held September 5 and 6 and were well attended. The Friday morning session was particularly concerned with developments and advances in industrial minerals with special emphasis on the Chicago area. The first two papers dealt with transportation on the Great Lakes and fuel movement into the Chicago area. The third paper proved to be of great interest, turning the spotlight on the fairly new hydraulic mining methods introduced by a silica company in the Ottawa, Ill. field.

Jan 1, 1952

Wabush Mines is the largest single supplier of iron ore to the Canadian steel industry, with 42% of its 6 million tpy of iron ore production going to the company's two Canadian owners-The Steel Co. of Canada and Dominion Foundries and Steel Ltd. Six other companies hold interests in Wabush Iron Co. Ltd. These are Lykes-Youngstown, Inland Steel Co., Intrerlake Steel Corp., Wheeling-Pittsburgh Steel Co., Finsider of Italy and Pickands Mather & Co. Field work on Wabush began in mid-1957 when a long-range program of economic, geologic, and metallurgical investigations started. This work was followed in 1959 by the construction of a temporary camp and a 700-tpd pilot plant. At the same time, work was also started on a 38-mi railway connection to Ross Bay, Newfoundland.

Jan 1, 1970

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

AN indication that Mesabi Range iron use companies may develop their own flotation processes for low grade iron ores is the report that Cleveland Cliffs Iron Co. is adopting a variation of one of the oldest known methods at its new Michigan treatment plant. Basically, the method involves using fatty acids and fuel oil reagents. The idea was developed many years ago and should be free of patent control. With other laboratories working on the same tack, it seems to be a pretty good bet that they will come up with their own processes. Any outside process will have to offer considerable advantage or low royalty rate to get consideration. Much of the appeal of the fatty acid process is the cheapness of the reagent. One source is pulp paper liquor in semi-refined form. With stream pollution legislation acting as a strong pressure, paper companies have been seeking ways to dispose of the material. Wisconsin has even attempted to use it for road binder.

Jan 5, 1953

By John J. Croston

The year 1935 witnessed one of the world's oldest industries—gold mining—attain the stature of a billion dollar business. Preliminary estimates indicate that somewhat over 30,000,000 oz. of gold was produced, the largest output ever recorded and exceeding the previous year by more than 11 per cent. Of this huge total the Witwatersrand field produced about 10,800,000 oz., compared with 10,480,000 oz. in 1934. Russia was apparently the stellar performer, and from incomplete data it appears that between five and five and a half million ounces were produced by the Soviets compared with 4,200,000 last year and 2,814,000 in 1933. The United States nosed Canada out of third place with a production of 3,546,000 oz. against 2,916,000 in 1934, while Canada increased her total from 2,965,000 to 3,291,000 oz. Similarly, gains of lesser magnitude were made in Australia, the Gold Coast and other countries. As a result of great activity in developing outlying areas on the Rand, and the great number of new companies building mills in Canada, Australia, the Gold Coast and the United States, the years 1936 and 1937 should see new high records, as these new producers will more than offset any decline in the older properties. The whole world has become "gold conscious" during the past three years. It has been the subject of innumerable articles by economists and others, but, unfortunately, because of their lack of actual mining knowledge, they have treated the production of gold as a static affair, ignoring geological and technical factors. It is hardly necessary to draw attention to the fact that the world's gold-mining industry was slowly but steadily shrinking in importance, owing to the gradual depletion of known deposits that were profitable to work at costs existing prior to 1929. The International Geological Congress at Pretoria and the League of Nations Committee drew attention to the estimates of the mining experts of the various governments predicting a steady falling off in world production. On the Rand there

Jan 1, 1937

By Howland Bancroft

This article is not presented as a treatise on tin mines and mining in Bolivia. It deals primarily with the tin situation, and but fragmentary information is given regarding individual properties, generalizations being necessary in so short an article. Data on general subjects related to tin mining in Bolivia are necessarily abbreviated and very incomplete. It is believed that the references to be found in this article will help those interested to a more thorough under-' standing of the general conditions extant in Bolivia. Bolivia produces from one-fifth to one-fourth of the world's supply of tin. The United States consumes about one-half of the world's supply and produces practically none. Tin ore is not reduced in the United States. These facts are not generally appreciated by American mining men. Many conflicting data have been published regarding tin in Bolivia. The Transactions of the Institute contain practically no mention of this subject.1 I have made a study of mines and mining conditions in the west coast republics of South America and have been particularly impressed by the possibilities of the Bolivian field.2 In consequence the thought seems justified that the present meeting would, present a fitting occasion to bring the tin situation in Bolivia to the attention of American mining men.

Jan 9, 1913

By A. C. Fieldner, W. A. Selvig

For purposes of coal classification it is desirable to know the composition and calorific value of the pure coal substance; that is, of the coal free from its ash-forming minerals. Two methods suggest themselves: (1) To free the coal from most of the ash-forming material previous to the analysis; and (2) to analyze the coal as received and calculate the analysis, with certain more or less arbitrary corrections, to the pure-coal basis. Calculation methods are obviously more apt to give correct results with low-ash than high-ash coals. With coals of unusually high ash it would appear preferable to remove, previous to the analysis, as much of the inorganic matter as possible, by float-and-sink or acid-treating methods. Effect of Ignition on Inorganic Constituents of Coal The need of corrections in calculating analysis to the pure-coal basis is due to the fact that the ash, as determined by ignition, is not the same, in either weight or composition, as the inorganic mineral matter in the coal. On ignition a number of changes occur in the coal such as loss of water of hydration of the shaly material, conversion of pyrite (FeS2) to ferric oxide (Fe203) with evolution of the sulfur as sulfur dioxide or possible fixation of more or less of the sulfur in the ash as calcium sulfate (CaSO4), and decomposition of calcite (CaC03) to calcium oxide (CaO). The amount of sulfur from pyrite which remains in the ash as calcium sulfate depends on the amount of calcite and pyrite in the coal. Certain coals high in both calcite and pyrite show relatively large amounts of sulfate sulfur in the coal ash. The determination of total carbon and hydrogen in coal includes, besides the organic carbon and hydrogen, the carbon of inorganic carbonates such as calcite, and the hydrogen of the water of composition of some of the ash-forming minerals. For detailed discussion of corrections proposed for calculations of coal analyses to the " pure "

Jan 1, 1930

By M. M. Singh, J. W. Brown

Three rocks of highly varied physical properties are selected for the first reported experimental study concerning microseismic activity of rock under tension to determine the effects of static fatigue, loading rate, repeated loading and rock anistropy compared to compression and bending loads. The microseismic method of detecting rock under deformation may be a great potential tool in surveillance and location in situ of dangerously stressed strata, as well as predicting rock failures. Noises emitted under load or the rate of energy (energy of noise pulses generated per unit time) are computed for varying conditions. The tests are conducted at constant load on a dead weight loading machine to eliminate all possible extraneous noises — an indispensable precaution — at various load levels. Experimental results are reported including the relation of total energy emitted to tensile strength of rock and the possibility of simulating a phenomenological model for microseismic activity. Plots of some of the experiments are included. INTRODUCTION Rock failure, whether on a large scale faulting in the earth's crust and rock bursts in mines, or on small scale ruptures of laboratory test specimens, generates transient vibrations in the rock mass. Mechanisms of intermittent deformation, such as twinning and cracking through and between mineral grains, also produce similar vibrations, but of very small amplitude. Such vibrations from both deformation and failure are referred to as microseismic activity, rock noise, or occasionally seismo-acoustical activity. An individual rock noise is sometimes

Jan 1, 1967

By G. R. Wilms

A study has been made of the structural changes in polycrystalline high purity aluminum during the tertiary stage of creep under conditions of constant tensile load. It appears that there is no basic modification in the particular mechanism of deformation that characterized the preceding secondary stage of creep, but that the changes in crystalline structure produced during the tertiary stage are only a consequence and not a cause of the accelerated strain. Intercrystalline fissures were observed on entry into the tertiary stage, and these might supplement the accelerated rate of strain owing to local stress concentrations. There is evidence that the formation of these fissures may be associated with the presence of surface imperfections, and it is suggested that a more generalized treatment of the results may explain certain creep characteristics of commercial alloys. IN previous work'-4 a study was made of the changes produced when specimens of annealed aluminum were deformed at various temperatures and rates of strain, especially under conditions leading to creep under constant tensile load. It was shown that, as the temperature was increased or as the rate of strain was decreased, elements of the substructure produced within the grains became coarser, and with the strain rate constant at a given temperature, their size tended to an equilibrium value. The preliminary process of the breaking down of the grains into a substructure was identified with primary creep.' The subsequent equilibrium, condition was associated with secondary creep. The question then arose whether the tertiary stage corresponded to any further significant change in the substructure. The question is also of interest in view of the opinion, expressed for instance by Andrade,5 that the tertiary stage is merely an accelerated rate of strain due to the reduced area of section of a specimen under continuous tensile load, and the other opinion, as suggested by the observation by Sully, Cale, and Willoughby6 of a tertiary stage in com-pressive loading, that this third stage is a real effect in its own right. The object of this paper is to record some observations on the tertiary stage of high purity aluminum. Experimental Procedure The material was aluminum of 99.98 pct purity as previously used. The specimens had a rectangular section of l/8 x l/2 in., and extensions were measured over a 1 in. gage length. After machining to shape, the specimens were annealed to give a standard grain size of 0.2 mm and then electropolished. The general procedure involved metallographic and X-ray diffraction examination at progressive stages of elongation (marked by arrows on the curves shown in Figs. 1 and 2), the specimen being extended to fracture under constant load at a given temperature. The X-ray tests were made by the back-reflection method from a stationary specimen, using CoK radiation. The longer edge of the micrographs in the paper corresponds to the direction of applied stress. Results The previous work showed that, in the secondary stage of creep in aluminum, three basic types of structure could be developed according to the temperature and rate of strain. These were: 1—slip, which predominated at the lower temperatures and higher rates of strain and produced the finest and least perfect substructure; 2—cell structure, which superseded slip as the temperature was raised and the rate of strain decreased and which was characterized by a coarser and more perfect structure and an absence of slip lines; and 3—a stage termed "boundary microflow," which predominated at still higher temperatures and lower rates of strain when the cell size had increased and become comparable

Jan 1, 1955

By Robert S. Dewey

Drilling in West Texas during 1942 was substantially less than in the previous year. In all. 1267 Wells were drilled, as compared with 2325 wells in 1941. Of these 1267 wells, 1052 oil wells, 10 gas wells and 69 dry holes were drilled in proven fields and 36 oil wells, one gas well and 99 dry holes were wildcat operations. Of the 36 wildcat wells completed as oil producers, 16 led to new field discoveries, three found new productive horizons in old fields, and 17 extended the productive limits of established fields. Where semiwildcat drilling took place along established productive trends, there was often no sharp demarcation between wildcat wells that extend field limits and normal development to fulfil lease obligations, other than the arbitrary classification of a well as a wildcat if it was drilled at a distance of 2 miles from a producing oil well. The dry hole drilled on the edge of a field may have proved a more hazardous operation than a semiwildcat drilled several miles from production but favorably located on structure. The percentage of successful wildcatting ranges from 26.5 down to 14 per cent, dependent upon the degree of inclusion of the semiwildcat operations. Irrespective of which figure was used, the West Texas area maintained its better than average exploratory position. No doubt a number of factors may have influenced the extent of the 1942 development. Among those arising from the economic dislocation attendant on the war effort, the following are worthy of note. Owing to inductions into the armed forces and shipyard competition for mechanically trained men, experienced drilling personnel was sharply reduced, thereby increasing drilling costs and well-completion hazards. Replacement labor has not met the same standard of responsibility or workmanship to which the oil industry has grown accustomed. Increased military consumption of aviation gasoline and other crude products, coupled with decreased domestic consumption of lower-octane gasoline, has stimulated the market demand for the types of sweet crude most readily processed with available refinery equipment to meet war requirements, and has depressed the market demand for the sour West Texas crudes. As a majority of the purchasers of West Texas crude normally ship a substantial portion of sour crude to the refineries on the Atlantic seaboard, the loss and diversion of tanker service between Gulf Coast and north Atlantic ports have further curtailed the market demand for this type of crude oil. As some purchasers of crude oil were able to move by pipe line their West Texas trunk-line capacity to Midwestern refining centers, they were not impelled to curtail purchases of West Texas crude. The varying ability of the purchasers of crude oil to market West Texas crude was reflected back to various fields to which they were connected, causing an unequal distribution of production as among fields and operators. The pipe-line runs from the West Texas-New Mexico area decreased from approximately 354,000 bbl. Per day in January to about 265,000 bbl. in December 1942. .Approximately 2,991,000 bbl. of West

Jan 1, 1943

By Robert S. Dewey

Drilling in West Texas during 1942 was substantially less than in the previous year. In all. 1267 Wells were drilled, as compared with 2325 wells in 1941. Of these 1267 wells, 1052 oil wells, 10 gas wells and 69 dry holes were drilled in proven fields and 36 oil wells, one gas well and 99 dry holes were wildcat operations. Of the 36 wildcat wells completed as oil producers, 16 led to new field discoveries, three found new productive horizons in old fields, and 17 extended the productive limits of established fields. Where semiwildcat drilling took place along established productive trends, there was often no sharp demarcation between wildcat wells that extend field limits and normal development to fulfil lease obligations, other than the arbitrary classification of a well as a wildcat if it was drilled at a distance of 2 miles from a producing oil well. The dry hole drilled on the edge of a field may have proved a more hazardous operation than a semiwildcat drilled several miles from production but favorably located on structure. The percentage of successful wildcatting ranges from 26.5 down to 14 per cent, dependent upon the degree of inclusion of the semiwildcat operations. Irrespective of which figure was used, the West Texas area maintained its better than average exploratory position. No doubt a number of factors may have influenced the extent of the 1942 development. Among those arising from the economic dislocation attendant on the war effort, the following are worthy of note. Owing to inductions into the armed forces and shipyard competition for mechanically trained men, experienced drilling personnel was sharply reduced, thereby increasing drilling costs and well-completion hazards. Replacement labor has not met the same standard of responsibility or workmanship to which the oil industry has grown accustomed. Increased military consumption of aviation gasoline and other crude products, coupled with decreased domestic consumption of lower-octane gasoline, has stimulated the market demand for the types of sweet crude most readily processed with available refinery equipment to meet war requirements, and has depressed the market demand for the sour West Texas crudes. As a majority of the purchasers of West Texas crude normally ship a substantial portion of sour crude to the refineries on the Atlantic seaboard, the loss and diversion of tanker service between Gulf Coast and north Atlantic ports have further curtailed the market demand for this type of crude oil. As some purchasers of crude oil were able to move by pipe line their West Texas trunk-line capacity to Midwestern refining centers, they were not impelled to curtail purchases of West Texas crude. The varying ability of the purchasers of crude oil to market West Texas crude was reflected back to various fields to which they were connected, causing an unequal distribution of production as among fields and operators. The pipe-line runs from the West Texas-New Mexico area decreased from approximately 354,000 bbl. Per day in January to about 265,000 bbl. in December 1942. .Approximately 2,991,000 bbl. of West

Jan 1, 1943

By Nicholas J. Grant, Hanna Ibach, Bill C. Giessen

The system Ta-Rh was investigated over the entire comnposition range using metallogvaphic and X-ray techniques as well as thermal analysis. Terminal solubility limits, solidus temperatures, and the crystal structures of two new intermediate phases were determined. There are five intermediate phases: o, tetragonal, isostructural with o(Fe-Cr); a1, orthorhomnbic : a2, orthorhombic, isostructural with CozSi; 0 3, a high -temperature phase of unknozun structure; and a TaRh3, cubic, AuCu3 structure. a, aL, a,, and a melt peritectically; and a TaRh, has a maximum melting point. Five peritectic and one eutectic reactions occur. THE Ta-Rh phase diagram has not been fully treated in the literature; however, two inter metallic phases have been described.&apos;-&apos; This study attempts to work out the diagram covering the details of phase boundaries as well as the crystallography of the intermediate phases. EXPERIMENTAL METHODS Starting materials were tantalum powder of 99.8 pct purity, supplied by National Research Corp., Cambridge, Mass., and rhodium powder of 99.9 pct purity, supplied by Bishop Co., Malvern, Pa. Analyses as given by the manufacturers are presented in Table I. In addition to the spectroscopic analysis, an oxygen analysis has been made of the tantalum powder. After preliminary trials, the standard procedure employed in making the alloys was as follows (see Ref. 4 for further details). The powders were weighed, mixed manually, compacted under 16,000 psi, and arc-melted at not more than 500 amp under thoroughly titanium gettered welding-grade argon of 400 mm Hg pressure. The gettering process was repeated after each melt. It had been shown previously5 that under these conditions no oxygen pick-up exceeding 0.001 pct in a hafnium button could be detected. The buttons, ranging from 5 to 10 g in weight, were inverted or, if possible, crushed and remelted three times. Melting presented no difficulty, except for tantalum-rich al- loys, which showed considerable spashing during melting. The average weight loss of 1 wt pct rose to 2.5 wt pct in these cases. Subsequent melting, however, resulted in losses of less than 0.1 wt pct. The melts obtained frequently showed small in-homogeneities, mostly in the tantalum-rich part of the system below 25 at. pct Rh. This was not due to insufficient blending of the elements, but to crystallization taking place from the cooled bottom. This condition was not improved by further re-melting; therefore the following precautions were taken. Cross sections of as-cast buttons were made. For the investigation only buttons were used where these inhomogeneities did not exceed 1 at. pct (estimated from the amounts of haSeS resent). In addition, only the center portions of such buttdns were utilized to minimize errors. Smaller buttons showed smaller concentration gradients and were used as a check. Finally, all alloys were homogenized to eliminate coring (see below). After this, the error in alloy composition due to inhomogeneity was cl at. pct. In order to confirm the concentrations of the alloys and to provide an impurity check, wet-chemical analyses and oxygen-fusion analyses of four key alloys were carried out. The results, together with the concentrations as calculated with the weight balance method, are presented in Table 11. It was found that for three alloys the agreement is very good (< 0.2

Jan 1, 1964

By J. Alfred Berger, O. M. Katz

The Zv-Hf-H ternary system was studied between 500° and 900°C at pressures less than 1 atm of hydrogen gas between 1 and 60 at. pct H. A new and unique microgravimentric apparatus was used. Cizanges of slope on pressure-hydrogen composition isothernis delineated phase boundaries. These boundaries separatecl the three regions, a, 0, and y—so designated to correspond to the regions of the Zr-H binary system—from the multiphased areas between them. A eutectoidal decomposition was found with the ß region phase or phases decornposing into a lamellar product on quenching to rool ter,zperatuve. Reproducible decomposition-pressure hysteresis occilrved lnainly at lower hydrogen cornpositions and at lower temperatures across multiplzase vegions between a and 0 and a and y. Tire effects of hqfniur7z on the hydriding charactevistics of zirconiurrz weYe as follows: 1) stabilization of the a and y vegions while destabilizing the 0 region; 2) a/?preciable elevation of the decomposition pressrkres in the multiphase region between the a and /3 field; 3) ~nouenzent of the eutectoid reaction to high te~nperatures; 4) reduction in the total qiiantity of hydrogen absorbed under one atmospheve of Hz p7-essure; and 5) introduction of a split deconzposilion at the eiitectoiclal poinl in pa?? of the ternavy. Assuru~ptions based on an ir-2terstitial vandonl-solulion rtioclel 0.f hydrogen in metals slzowed that the bindit~g energy between solute sites prednnzinatecl at low /i?!dvogen concentrations. However, at high hydrogen contents the entropy was the predorninatlt factor in determining the stability of the Zr-Hf-H al1o.s. This was interpreted to mean a scarcity of filrtlzer itltevslilinl solute sites caused by hydrogen-hydvogen intet-actions in the metal lattice. INTEREST in the reaction of hydrogen with metals has increased in the past few years for the following reasons: 1) the formation or use of high hydrogen potential environments in nuclear reactors; 2) the reaction of hydrogen with alloys in nuclear reactors with the accompanying deleterious effects on the mechanical and corrosion properties; 3) the theoretical implications of thermodynamic data on the theory and rules of alloy formation in the metal-hydrogen systems; 4) the use of hydrogen-containing fuels in rocket engines; 5) the need for a process of making fine metal powders of high-melting reactive metals; and 6) the beneficial impregnation of superconducting alloys with hydrogen. In nuclear pressurized-water reactors, the problem exists of limiting the hydrogen pickup of zirconium alloys which are utilized as fuel cladding, heat shields, and support members. In general, zirconium alloys have good mechanical and corrosion-resistant properties in high-temperature water. However, hydrogen is absorbed from the corrosion reaction between metal and water, greatly accelerating the formation of the corrosion product ZrOz as well as mechanically embrittling the underlying metal. In addition, recent observations1 at zirconium to hafnium welds showed that secondary elements in zirconium can have an appreciable, and somewhat unexpected, effect on hydrogen absorption. This paper lists the thermochemical data in the range 500" to 900°C for the equilibrium reaction of four high-purity Zr-Hf alloys with hydrogen. Phase boundaries and thermodynamic functions are determined while the structural data will be presented in a future paper. In general, the Zr-Hf-H system approximates the well-known, eutectoidal, Zr-H diagram2,3 with modifications introduced through the behavior of hafnium.4,5 The Hf-H system,&apos; published while this work was in progress, provided a consistent trend with the Zr-Hf-H data. PREPARATION OF Zr-Hf ALLOYS Table I presents a complete flow chart of the preparation procedure. The zirconium and hafnium crystal bars were completely immersed in high-purity kerosene and slowly cut into thin wafers. Wafers were then cold-sheared into approximately 1-g pieces, thoroughly cleaned, weighed, and inserted into the furnace. The alloys, B-2, B-4, B-6, and B-8, were then nonconsumable arc-melted under 500 mm of purified argon. Additional purification of the argon was accomplished by melting a large titanium button each time an alloy was re-melted or a different alloy melted. Each alloy button, which weighed 25 g, was remelted four times in an approach to complete homogeneity. Material losses were less than 0.02 wt pct. Alloy buttons were alternately cold-rolled and vacuum-annealed into 10- and 20-mil sheets. Table I1 gives the composition of the four alloys used. Very little elemental segregation existed be-

Jan 1, 1965

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline&apos; and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

By S. W. Parr

FROM a study of sulfur with reference to its specific combination in coal, published as University of Illinois Bulletin No. 111, 1919, it is now possible to determine the various forms of this constituent with a good degree of accuracy. This fact suggests two questions: (1) Are the same analytic methods applicable to coke? (2) Is there any correlation between the forms of sulfur as it occurs in coal and the residual sulfur found in the finished coke? The answer to the second question might be helpful in answering a still further question as to what chemical route the sulfur travels during the carbonization process. While the special studies along these several lines are by no means complete, a few preliminary statements are herewith presented. They may, at least, prove suggestive of further possibilities from a continuation of research along these lines. There is no reason, chemically, why the analytic methods devised for coal should not apply to coke and a fair amount of experience in connection with such use affords confirmation of this statement. The procedure in the case of coal may be briefly outlined as follows; Combinations of sulfur as sulfate, or sulfides other than FeS2, are readily dissolved without disturbing either the pyrite sulfur or the sulfur that is in organic combination by means of dilute hydrochloric, acid-1 part of concentrated HC1 to 10 parts of water or approximately 3 per cent. acid. Digestion at 60° C. for 24 hr. insures the complete removal of the sulfur thus combined. In freshly mined coal the amount of such sulfur is very small; weathering processes, however, may very materially increase the amount of sulfate present.

Jan 9, 1919

By A. D. Schwope, L. R. Jackson, K. F. Smith

Burghoff and Blank1 have pointed out that the creep properties of hard-drawn coppers are closely associated with their individual softening characteristics and have further shown that the creep resistance of various types of copper is improved, under certain circumstances, by cold stretching. In the design of certain types of electrical machinery, it is important to have the creep resistance as high as possible; furthermore, short-time creep strength is important since in many cases stresses are large only during warming-up and cooling-down periods. In this paper, data are presented showing the effect of cold work on the short time creep strengths of various types of commercial copper under several conditions. It is shown that trends from short-time creep tests are evident at longer times. Materials Used in the Investigation The coppers used in this investigation were commercial grade and of two basic types, oxygen free high conductivity (OFHC) and tough pitch. Additions of silver in amounts of 15 and 25 oz per ton were added to each of the two coppers. The analyses of these six coppers are given in Table 1. Originally, they started as wire bars 4 X 4 X 54 in. A. square rod was made by hot rolling the wire bars to 9/16-in. rod in 8 passes. This rod was then cold drawn to 0.445-in.-diam rod and annealed for 3 1/2 hr at 1000°F. It was then cold drawn to 0.325-in. rod and again annealed at 1000°F for 3 1/2 hr. Hard square rods were then made by cold rolling to 0.257 X 0.257-in. rod. Soft wire was made from the hard- drawn material by annealing at 650°F for 3 hr. The final rolling was performed using a set of 9-in. grooved rolls revolving at 30 rpm, which produced square wires. Reductions of approximately 5, 20, 30, and 40 pct were obtained using several passes in the same direction for the large reductions. The 5 pct reduction by drawing was accomplished using a steel die having 2 parallel bearing surfaces. The die angle was 7 1/2 degrees and the wires were lubricated with a paste of ceresin wax dissolved in carbon tetrachloride. The speed of drawing was 13 fpm. Since work was done on only two sides of the wire simultaneously, it was necessary to rotate it 90 degrees each pass to insure uniform deformation. The room-temperature tensile properties of the various tempers are given in Table 2. The grain size of the an- nealed 0.257-in. wires was uniform and averaged about 0.035-0.045 mm. Experimental Procedures for Short-time Creep Tests Standard creep-test frames (Fig 1) were used for the testing. Special fixtures were designed to apply axial compressive and tensile loads to the copper wires. The compression specimens were 1 in. long and the ends were ground flat and parallel. The creep in compression was indicated by the movement of reference marks s-ratched on intersliding platinum strips attached to the moving heads of the fixture. The movement was measured with an optical micrometer fitted with a filar eyepiece on which the smallest division was 0.00005 in. The tensile creep specirriens were 4 in. long which provided ample gripping surface for the jaw-type grips. The platinum strips were attached to a one-inch gauge length of the wire and the creep measured as previously described. The single-specimen furnaces were connected to individual power and control sources. The controlling equipment consisted of Foxboro controllers

Jan 1, 1950

A. W. TRACY&apos; AND D. H. THOMPSON (presented in written form).-Messrs. Ed¬munds, Anderson and Waring are to be commended for their excellent work in so painstakingly reducing to constants, the variables believed to be associated with these types of stress corrosion. An ammonia stress-cracking apparatus similar in many respects to the one described has been assembled. Certain aspects of its construction may be of interest. Tensile loading of the specimens, which are usually Y8-in. diameter wires, is accomplished by springs acting in compression in compact, portable, tubular assemblies weighing less than 10 lb. The lower end of each assembly contains the test specimen and is passed into the test chamber for exposure to the moist ammoniacal atmosphere. There is considerable convenience in being able to load the specimens in a portable unit, which may be warmed to prevent condensation, and then thrust instantaneously into the test chamber. Spring loading obviates the use of weights, but it has the disadvantage of allowing some relaxation of the load if the specimen elongates during corrosion. The maximum loss in load found so far was 20 per cent. The air supplied to the test chamber is humidified by passing it through thermo¬statically controlled water. The air is dispersed into fine bubbles by being forced through a porous ceramic filter at the bottom of a tank containing about 10 liters of water. The temperature of the water is controlled independently of the tempera¬ture of the test chamber. Thus, with the

Jan 1, 1945

By M. E. Wadsworth, R. C. Peterson, W. M. Fassell

The temperature and pressure dependence of the reaction of tantalum in oxygen were investigated from 500° to 1000°C at pressures from 10 mm Hg to 600 psi total oxygen pressure. Tantalum was found to oxidize linearly under the above conditions. Three distinct regions of temperature dependence were found with different energies of activation. From 500° to 600°C the rate of oxidation of tantalum was found to be essentially independent of the oxygen pressure at the pressure investigated. The oxidation rate increases rapidly with an increase in pressure from 600&apos; to 800°C. The dependence of the oxidation rate on the bulk concentration may be expressed by V = k&apos;?, where k&apos; is the specific rate constant and ?=k1Co2/(l + K1Co2), where k, is the equilibrium constant for the adsorption of oxygen on tantalum. ONLY a limited amount of data has been presented in the literature on the oxidation behavior of tantalum metal. Some values of its oxidation rate were reported in the Corroston Handbook&apos; and by McAdams and Geil.&apos; The first extensive investigation of tantalum was the work of Gulbransen and Andrews." They determined the reaction rates of tantalum in O2 and N2. Their results indicate that this metal follows the parabolic law in the temperature range of 250" to 450°C in O2 at pressures of 7.6 cm Hg with an activation energy of 27,400 cal per mol. In nitrogen, the metal follows the parabolic law from 500" to 800°C at 7.6 cm pressure. All experimental determinations were of 2 hr or less duration and deviations from the parabolic rate conceivably could occur at longer times. A spectrophotometric study of the oxidation of tantalum by Waber, Sturdy, Wise, and Tipton&apos; indicated good agreement between this method and the microbalance technique. The experiments were conducted in air from 220" to 350°C. The metal was found to follow the logarithmic law up to 320°C and the parabolic law at higher temperatures. The activation energies in the logarithmic region were reported as 12.57 kcal per mol and 12.0 kcal per mol, respectively, for the microgravimetric and spectrophotometric methods. In the parabolic region the activation energy was found to be 27.2 kcal per mol, in good agreement with the value of Gulbransen and Andrews." The present paper is concerned with the behavior of tantalum from 500" to 1000°C in oxygen at pressures ranging from 1/2 to 40.8 atm pressure. Earlier preliminary data by McKewan5,6 indicated the following facts concerning the behavior of tantalum: 1—At temperatures from 500" to 600°C, the metal followed the linear law. 2—At 575°C the rate of oxidation was found to increase with O2 pressure. 3—The Arrhenius plot in this temperature region was nonlinear. The nonlinearity of the Arrhenius plot was indicative of a more complex behavior than originally suspected for this metal.

Jan 1, 1955

By L. Larson

SMELTERMEN in the copper industry know that punching the tuyeres of a copper converter is a difficult, disagreeable, and at times a hazardous job. Knowing this, many men in the industry have given serious consideration to punching by mechanical means. As evidence of such consideration, a great many patents have been issued covering various mechanical devices or machines for doing this task. In 1942, as war-created manpower shortages became more acute, it became increasingly difficult to get men to punch tuyeres. Faced with this situation at the McGill smelter, it was decided that an all-out effort should be made to develop some sort of a mechanical punching device. The various patents were studied over thoroughly but none of the devices seemed suitable, all were discarded and it was decided to develop one, using the ideas of the personnel at McGill. Initial test work indicated that a separate punching device should be attached to each tuyere. This meant that an adapter would have to be developed which would accommodate such a device; the adapter to be so constructed that it could be substituted for the regular Dyblie valve head, and be punched either by mechanical means or by hand. Also a method for quickly attaching or detaching the punching unit would have to be devised. If the punching unit was attached to the adapter, then the punch rod and tip would have to remain inside of and reciprocate within the tuyere pipe. This last requirement meant that the punching device, the adapter, the piston rod, and punch rod must be in perfect alignment. The whole arrangement thus would become an integral part of the converter and would rotate along with the tuyere line to all the positions required for converter operation. If the puncher was to rotate with the converter, there was also a problem of limited clearance. The construction of a device to meet all of these conditions imposed many problems. In the latter part of 1942, two pieces of equipment were constructed and tried out under test-stand conditions. Both of these devices were very crude, but test-stand operation indicated that progress was being made. Neither of the units was considered good enough to be attached to and tried out on a tuyere of an operating converter. In May 1943, work was started on another device and in August of that year it was attached to and actually punched a single tuyere of a converter on an experimental basis (fig. 1). This unit was essentially a cylinder 3 in. in diam and about 15 in. long inside. Valve ports were so located as to provide a 1-in. cushion on each end of the stroke. The cylinder ports were piped to a 3/4-in. four-way disk valve. High pressure air (90 psi) was delivered to the valve by means of a long hose, thus making it possible to supply air to the device at all operating positions of the converter. The forward and return punching strokes were accomplished by shifting the valve handle as required. With the 3/4-in. valve, stroke velocities from 15 to 18 fps were achieved. Punching with this experimental arrangement was carried on for some time, but many difficulties were encountered. The punch rod tips often stuck in the tuyere accretion, indicating that more energy of some sort was necessary to avoid sticking the punch rod. To overcome sticking, experiments continued with a speeded up unit and although progress was made, troubles of various kinds continued to appear. On this unit, piston cup seals passed the valve ports which proved to be of very poor construction. Also the piston, driven forward at approximately 28 fps, would often bottom metal to metal in the forward end of the cylinder causing both mechanical and operational trouble. Sometimes the punch rod and at other times the piston rod would break loose and be shot through the tuyere pipe into the converter. Bottoming and poor timing of valve reversal caused a bounce and a hesitation at the end of the forward stroke, with the result that the punch rod

Jan 1, 1951