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By R. C. Hall

The magnetic anisotropy and magnetostriction of single crystals of alloys between 25 and 59 wt pct Co in Fe have been determined in the disordered and ordered states. The magrzetostriction is large and positive for all alloys in both states of order (up to 150 x 10-6 for A,, and 40 x 10-6 for 111). The magnetic anisotropy becomes zero rzear 41 pct Co for the disordered state. Ordering shifts the zero-anisotropy composition to about 50 pct Co. COBALT-iron alloys have for many years been of interest as magnetic materials because they have unusually high magnetic saturation values.' This interest was increased recently by the development of Supermendur.' Supermendur is an alloy of 49 pct Co-49 pct Fe-2 pct V* which was found by suitable purification and heat treatments, including a magnetic anneal, to possess excellent magnetic properties. These included a square hysteresis loop with a low coercive force and a high magnetization, and a low total loss. Two factors which are important in determining the magnetic hysteresis properties are the basic magnetic properties of magnetostriction and anisotropy. Alloys having zero anisotropy and zero magnetostriction show improved hysteresis properties.3 Since very meager data4-' are available in the literature on the single-crystal anisotropy and magnetostriction of the cobalt-iron alloys, the present program was undertaken to determine these two properties in the disordered and ordered states. EXPERIMENTAL TECHNIQUES Ingots of the cobalt-iron alloys containing from 25 pct to 59 pct Co in iron were vacuum melted from electrolytic iron and cobalt of 99.9 pct purity. The ingots were cooled at a rate of about 1°C per hr through the transformation temperature (950" to 980°C dependent on the alloy content) for the growth of large grains. From these grains, single-crystal disks were fabricated with either the (110) or (100) plane parallel to the faces of the disk. The crystals were given two heat treatments to produce either the ordered state (cooling rate of 20°C per hr from 850 "C) or the disordered state (water quench from 850 °C). Since the iron-cobalt alloys order very rapidly, the water quench may not have produced complete disorder in all cases. Due to the method of growth, the crystals were not perfect. Most of the samples had low-angle boundaries and a few had some small included grains. These imperfections could and probably did affect the accuracy of both the magnetic anisotropy and magnetostriction measurements. Much of the scatter in the data may be attributed to the crystal imperfections. The methods of determining the spontaneous saturation magnetostriction and the anisotropy have been previously described.419110 MAGNETOSTRICTION The magnetostriction in the [loo] and [Ill] directions (hO0 and ?111 respectively) is illustrated in Fig. 1 for the disordered state. Both ?100 and ?111i became large positive values as cobalt was added to iron. The state of order did not have a large effect on the magnetostriction. The effect of order did not appear too consistent in these data. Tentative curves are shown in Fig. 1 for the ordered magnetostriction near the FeCo composition; here ?100 appeared to be lowered and ?111 raised as the degree of order was increased. These results agree qualitatively with the

Jan 1, 1961

MINING AND METALLURGICAL SOCIETY OF AMERICA San Francisco Section The San Francisco Section of the Mining and Metallurgical Society of America held a joint meeting with the local section of the American Institute of Mining Engineers at the Engineers' Club, San Francisco, on Tuesday, Apr. 16, 1918. The meeting was preceded by a dinner. Letters from the parent body in NewYork asking for the consideration of the proposed bill before Congress, and an expression of opinion relative to the appointment of a Federal Administrator of Mines justified the joint meeting of the local sections of the two mining societies, in that a more representative opinion of the engineers of California could he obtained. The meeting was called to order at 7:15 P.M. by Mr. Frank H. Probert acting as Chairman. About thirty engineers were present. Mr. Probert read a letter of March 14, from Secretary Huntoon, asking that the meeting be called. He read excerpts from Bulletin 117 of February 28, 1918, of the Mining and Metallurgical Society containing a copy of the proposed bill, so that all present might be advised of its essential contents. He briefly commented on the urgent need of such legislation and invited discussion of the subject. After long and thorough discussion on the part of the members present, Professor Lawson made the following motion: I move that a resolution expressing the sense of the joint meeting of the local sections of the American Institute of Mining Engineers and Mining and Metallurgical Society of America be forwarded to the secretaries of the two societies to the effect that we heartily approve of the purpose and intention of the bill designed to promote and stimulate the production of minerals necessary for the successful prosecution of the war; and that we suggest prices should be fixed for the period of the war and two years thereafter, and that these prices, guaranteed by the Government, should apply at the nearest shipping point to place of production of the minerals. This motion was carried. The meeting then adjourned, and a telegram was sent by Mr. Probert, the Chairman, to Mr. Huntoon, notifying him of the motion that had been carried at the meeting.

Jan 7, 1918

By J. S. Hromatko, L. J. Gurevich

In the course of the examination, at the BureLu of Standards, of fusible tin boiler plugs for the Steamboat Inspection Service, it became evident that an investigation should be undcrtaken to determine the precautions necessary in the manufacture of acceptable plugs. The results of the tests of these plugs show that their manufacture has improved, though at present not all of the plugs tested are, satisfactory. Table 1 gives the result of tests of some 1500 plugs from about 100 makers. Records of the tests show that several of the makers were able to produce satisfactory plugs with every pouring. The Steamboat Inspection Service has the following specifications for fusible plugs: "Fusible plugs for use in boilers of steam vessels under the jurisdiction of the Steamboat Inspection Service shall be made of bronze casing with the bore tapering continuously and openly from end to end, and filled from end to end with tin not less than 99.7 per cent. pure and to contain not more than 0.1 per cent. of lead and not more than 0.1 per cent. of zinc. The small end of the bore may be countersunk not more than 1/32 in. in depth and width, but no recess, thread, or cavity other than this countersink shall be allowed." Table 1.—Thirty-"five-mdh Testing Record of Fusible Plugs Causes of Rejection Inspection Period June-November, 1916.................. 311 32.8 47.2 3.8 11.5 15. 1 10.9 1 1.9 4.5 December, 1916-May, 1917............. 318 71.4 28.6 2.2 4.4 12.8 5.9 i ... 2.8 June-November, 1917.................. 228 73.0 27.01 ... 9.6, 5.2 9.6' ... 0.8 December, 1917-May. 1918............. 214 72.028.0 0.9 0.4 11.6 7.0 ... 7.9 June-November, 1918...............250 70.7 29.3 ... 2.0 20.0 5.2 ....2.8 December, 1918-April. 1919............ 23378.121.9 7.2 1.2 1 4.7 3.0 ... 6.0 Total 35 months....................1544.69.7 30.3 2.3 4.8 11 0 6.9 0.3 4.1

Jan 1, 1921

By Albert Sauveur

As director of the Division of Metallurgy of the Technical Section of the Air Service, American Expeditionary Forces, from August, 1917, to January, 1919, I devoted much time to the study of the steels best suited to the construction of aircraft. It became apparent at a very early stage of my investigation that the practice of builders varied greatly in regard to the number of different steels to be used, to the kinds of steels, and to their treatment. Some manufacturers employed as many as fifteen steels while the builder of one of the newest motors, favorably passed upon in the United States, assured me that two or, at the most, three kinds of steel was all he needed to produce satisfactory results. In the matter of treatment, the manufacturers were also greatly at variance.. Some treated their steel with considerable refinement, while others paid but scant attention to this feature. Some manufacturers case-hardened many parts, while others used the case-hardening process sparingly, if at all. Nickel-chromium steels were used at some works for case-hardening while at other plants this treatment was applied exclusively to carbon steels. Air-hardening nickel-chromium steel was used extensively by some and not at all by others. Considerable variance existed likewise in regard to the steels used for admission and exhaust valves. The conclusion was obvious, that no two manufacturers of airplane motors held like opinions as to the steels to be used or as to the treatment they should receive. Was it to be inferred from this that the many committees and associations that had been created, in part at least, for the standardization of aircraft steels had failed to make proper recommendations or that the manufacturers had ignored their recommendations? Confining our inquiry to the committees and associations that had dealt with this question in England, France, and the United States, it was found that in Great Britain the British Engineering Standards Committee, now the British Engineering Standards Association, had devoted much time to the problem of satisfactory standards for aircraft steels. In April, 1918, this Association presented a set of specifications

Jan 9, 1919

By Edward Pesout

The McGill smelter started operations in the year 1907. The smelter furnaces were fired with run-of-mine coal on grates until April 1911, when oil firing was introduced. Oil firing continued until April 1918, when the initial coal-pulverizing plant was started.' Early Pulverizing Plant Various alterations were made to that plant during its operation, one of the more important being in connection with the system for delivering pulverized coal. In order to minimize coal-dust explosions and fires, the return portion of the main delivery line was eliminated in the year 1928. Thereafter coal-dust explosions and fires were greatly reduced. Pulverized coal was prepared at this plant primarily for the reverberatory furnaces, but for several years it was also delivered to the converting plant, roasters and power-plant boilers by a system of auxiliary fans and delivery lines. During the period March 29 to April 8, 1929, one reverberatory furnace was fired with pulverized coal produced by an Aero, type J, unit coal pulverizer with a rated capacity of 5 tons per hour. This machine actually pulverized its rated capacity but the product was too coarse. After certain regulations, a her product was obtained but the pulverizer capacity decreased and this resulted in insufficient coal for efficient furnace operation. Table I gives a comparison of the average screen analyses of the pulverized-coal products from the impact-type unit pulverizer and the regular coal-plant installation. It was definitely proved that this size and type of unit pulverizer could not furnish sufficient coal of proper fineness to give smelting results comparable to that obtained with the regular coal-pulverizing plant. The coal from this unit pulverizer was so coarse that it did not ignite or burn properly and thus did not produce the proper heat for efficient smelting. During the latter part of 1929 and the early part of 1930, experimental work was conducted with a 7-ft. o-in. by 48-in. Hardinge conical ball-mill coal-grinding unit, which was installed alongside a furnace in the reverberatory building. Results obtained from the test run indicated that this unit would furnish sufficient coal of proper fineness for good smelting.

Jan 1, 1947

By Edward Pesout

The McGill smelter started operations in the year 1907. The smelter furnaces were fired with run-of-mine coal on grates until April 1911, when oil firing was introduced. Oil firing continued until April 1918, when the initial coal-pulverizing plant was started.' Early Pulverizing Plant Various alterations were made to that plant during its operation, one of the more important being in connection with the system for delivering pulverized coal. In order to minimize coal-dust explosions and fires, the return portion of the main delivery line was eliminated in the year 1928. Thereafter coal-dust explosions and fires were greatly reduced. Pulverized coal was prepared at this plant primarily for the reverberatory furnaces, but for several years it was also delivered to the converting plant, roasters and power-plant boilers by a system of auxiliary fans and delivery lines. During the period March 29 to April 8, 1929, one reverberatory furnace was fired with pulverized coal produced by an Aero, type J, unit coal pulverizer with a rated capacity of 5 tons per hour. This machine actually pulverized its rated capacity but the product was too coarse. After certain regulations, a her product was obtained but the pulverizer capacity decreased and this resulted in insufficient coal for efficient furnace operation. Table I gives a comparison of the average screen analyses of the pulverized-coal products from the impact-type unit pulverizer and the regular coal-plant installation. It was definitely proved that this size and type of unit pulverizer could not furnish sufficient coal of proper fineness to give smelting results comparable to that obtained with the regular coal-pulverizing plant. The coal from this unit pulverizer was so coarse that it did not ignite or burn properly and thus did not produce the proper heat for efficient smelting. During the latter part of 1929 and the early part of 1930, experimental work was conducted with a 7-ft. o-in. by 48-in. Hardinge conical ball-mill coal-grinding unit, which was installed alongside a furnace in the reverberatory building. Results obtained from the test run indicated that this unit would furnish sufficient coal of proper fineness for good smelting.

Jan 1, 1947

By Edward Pesout

THE McGill smelter started operations in the year 1907. The smelter furnaces were fired with run-of-mine coal on grates until April 1911, when oil firing was introduced. Oil firing continued until April 1918, when the initial coal-pulverizing plant was started.1 EARLY PULVERIZING PLANT Various alterations were made to that plant during its operation, one of the more important being in connection with the system for delivering pulverized coal. In order to minimize coal-dust explosions and fires, the return portion of the main delivery line was eliminated in the year 1928. Thereafter coal-dust explosions and fires were greatly reduced. Pulverized coal was prepared at this plant primarily for the reverberatory furnaces, but for several years it was also delivered to the converting plant, roasters and power-plant boilers by a system of auxiliary fans and delivery lines. During the period March 29 to April 8, 1929, one reverberatory furnace was fired with pulverized coal produced by an Aero, type J, unit coal pulverizer with a rated capacity of 5 tons per hour. This machine actually pulverized its rated capacity but the product was too coarse. After certain regulations, a finer product was obtained but the pulverizer capacity decreased and this resulted in insufficient coal for efficient furnace operation. Table I gives a comparison of the average screen analyses of the pulverized-coal products from the impact-type unit pulverizer and the regular coal-plant installation. [ ] It was definitely proved that this size and type of unit pulverizer could not furnish sufficient coal of proper fineness to give smelting results comparable to that obtained with the regular coal-pulverizing plant. The coal from this unit pulverizer was so coarse that it did not ignite or burn properly and thus did not produce the proper heat for efficient smelting. During the latter part of 1929 and the early part of 1930, experimental work was conducted with a 7-ft. 0-in. by 48-in. Hardinge conical ball-mill coal-grinding unit, which was installed alongside a furnace in the reverberatory building. Results obtained from the test run indicated that this unit would furnish sufficient coal of proper fineness for good smelting.

Jan 1, 1945

By H. M. Warrren

IN the past, steam engines were used in practically all cases for driving the machinery, in and about an anthracite breaker, and hence little or no accurate data were available as to the power requirements for starting and operating the individual machines, which make up the complete equipment. It was impossible to segregate the power necessary to drive each individual machine, first, because the equipment was driven in groups, and second, because it was impracticable to obtain graphic, integrated, or instantaneous records of the horsepower used. As a result of these conditions, it was found, when individual electric motors were applied to the various machines, that more accurate and complete data were needed in order to provide motors of the proper power and design for the particular services to be rendered. In order to obtain the desired information, the writers made and collected a number of tests, from time to time, on the individual motor drives in- electrically operated breakers, and as these tests have been of great value, it occurred to them that a paper giving the results might be of service to other engineers interested in similar installations. Table I shows the .results of these tests. All the motors tested were of the three-phase, 60-cycle, 440-volt, induction, squirrel-cage type, except a few, which, on account of size and starting conditions, were of the wound-rotor type. The instruments used in making these tests were: An integrating watt-hour meter, a graphic ammeter, and a graphic voltmeter. These instruments were connected in each motor circuit, and a record of a day's run of 9 hours was obtained from each machine. From these tests, the running light load, the average all-clay load, and the instantaneous peak readings in amperes, volts, and kilowatt input, were obtained. By means of the characteristic curves obtained from these motors at the factory, the power factor, the efficiency, and the horsepower output were calculated for each particular test. Starting tests were made by the brake-arm method, in which the torque in pounds was measured directly on a spring balance.

Jan 2, 1916

By H. M. Warren, E. J. Powell, A. S. Biesecker

In the past, steam engines were used in practically all cases for driving the machinery in and about an anthracite breaker, and hence few or no accurate data were available as to the power requirements for starting and operating the individual machines, which make up the complete equipment. It was impossible to segregate the power necessary to drive each individual machine, first, because the equipment was driven in groups, and second, because it was impracticable to obtain graphic, integrated, or instantaneous records of the horsepower used. As a result of these conditions, it was found, when individual electric motors were applied to the various machines, that more accurate and complete data were needed in order to provide motors of the proper power and design for the particular services to be rendered. In order to obtain the desired information, the writers made and collected a number of tests, from time to time, on the individual motor drives in electrically operated breakers, and as these tests have been of great value, it occurred to them that a paper giving the results might be of service to other engineers interested in similar installations. Table I shows the results of these tests. All the motors tested were of the three-phase, 60-cycle, 440-volt, induction, squirrel-cage type, except a few, which, on account of size and starting conditions, were of the wound-rotor type. The instruments used in making these tests were: An integrating watt-hour meter, a graphic ammeter, and a graphic voltmeter. These instruments were connected in each motor circuit, and a record of a day's run of 9 hours was obtained from each machine. From these tests, the running light load, the average all-day load, and the instantaneous peak readings in amperes, volts, and kilowatt input, were obtained. By means of the characteristic curves obtained from these motors at the factory, the power factor, the efficiency, and the horsepower output were calculated for each particular test. Starting tests were made by the brake-arm method, in which the torque in pounds was measured directly on a spring balance.

Jan 1, 1916

By R. A. Liddle

Intermitt'en'I'ly during the past 10 years showings of oil and gas in tests drilled in the eastern part of Texas have stimulated the search for production. Tests on the flanks of the long-known salt domes, principally Keechi and Butler, have found oil in small quantity in the Woodbine formation of the basal part of the Upper Cretacrous. In the central part of Cherokee County, Colliton et all in 1926, in their Clapp No. 2 found a good showing of 37" B6. oil at about 3500 ft. Several wells were drilled in 1926 and 1927 as a result of this showing. On Jan. 22, 1927, Humble Oil & Refining Co. wildcatting on Carey Lake salt dome, obtained commercial production in its Clark No. 1. This inaugurated intensive exploration both for salt domes and for other types of structure. As a result several new domes and a few promising structures of other types have been discovered. Development in East Texas durinG 1927 Carey Lake Dome Location.—On the Neches River in Anderson and Cherokree counties, 10 miles west of Jacksonville, Cherokec (lounty. (Fig. 1.) date of Discovery.—During 1925 geologisls of the Humble Oil & Refining Co. working in the Neches River valley discovered slight surface fracturexs, cratic dips, and slickensided clays and sands in green-sands of the Mount Selman formation north of Carey Lake. A number of core tests were drilled by the Humble Oil & Refining C'o. during 1925 and 1926, some more than 1500 ft. deep, to check their surface obsuvations of faulting, and the possibilities of a salt dome. On May 16, 1927, solid rock salt was reached at 2142ft. in the first deep test on the prospect. Surfacc Indications.—Surface indications of the Carey Lake dome, though not as evident as manifestations at the previously known domes of Palestine, Keechi, Butler, Grand Saline, Steen and Brooks, are more noticeable than on any of the domes discovered in 1927. F. E. Poulsen, of the Pure Oil Co., who examined the area before the deep tests were drilled, noted the alignment of erratic surface dips which suggested faulting, especially in conjunction with slickensiding, and the local deflec-

Jan 1, 1928

By Dwight H. Seely, Louis R. Records

A process for low-temperature dehydration of natural gas utilizing Joule-Thomson effect in expansion through a throttling orifice has been tested in a full-scale field installation. The results of these tests are presented in the form of performance curves from which the process may be easily evaluated. The effect of separation temperature on condensate recovery from the process is also shown. INTRODUCTION The transportation of natural gas from producing well to the consumer has always encountered the problem of hydrate prevention. This problem has become increasingly important in the past ten years due to the rapid increase in produced gas volumes, production pressures, transportation pressures and distance from producing wells to consumer. Natural gas, as normally produced from gas or gas-condensate wells, is saturated with water vapor at well-head conditions of temuerature and pressure. The solution of the hydrate problem require; but one basic process — dehydration of the gas to a water content which will result in a water dew-point below the minimum temperature to be encountered from the producing well to the point of consumption. Much of the recent development of gas and gas-condensate reserves in the Gulf Coast Area has been in locations which are accessible only by water. High well-head pressures, pipeline construction and maintenance costs and the desirability of final central gas-condensate separation facilities have stimulated the development of dehydration equipment which can be installed at each well and which will permit hydrate-free transportation of both gas and condensate in the same line to central facilities. There are four types of natural gas dehydration processes now used: 1. Adsorptive processes. 2. Absorptive processes. 3. Chemical reaction processes. 4. Refrigeration processes. The first three of these processes are indirect in that they require use of adsorbents, absorbents or reactive chemicals. These materials require regeneration and part of the total gas stream is consumed in the regenerative process. Indirect processes have a wide range of flexibility as defined by allowable operating pressure and temperature, but most are not easily adapted to automatic operation. The refrigeration process described in this paper was designed for installation at the producing well-head. It requires no regenerative cycle and with normal well-head temperatures no external source of heat. The flexibility of this process is limited only by the pressure drop which may be allowed between well-head and transportation line. THEORY There are three basic physical concepts involved in the low temperature dehydration process. These are: 1. Formation of hydrocarbon hydrates. 2. Joule-Thompson effect resulting from the expansion of gaseous mixtures through a throttling orifice. 3. The equilibrium composition characteristics of water vapor and gaseous hydrocarbon mixture.. The chemical composition and physical structure of hydrate; have been described by several investigators.3,4,5,10 Specific conditions of temperature, pressure and composition as well as the requirements for turbulence and presence of free water necessary for hydrate formation have been described by Katz.6 Natural gas hydrates, as they are found in plugged gas pipe lines, have the appearance of packed snow. The mass of these hydrates has low continuous porosity and permeability. Joule-Thomson effect. or the reduction in temperature which occurs when natural gas is throttled throusll a restrictive orifice, is the basic phenomenon which permits efficient use of refrigeration for the purpose of dehydrating natural gas. Joule-Thomson coefficients for gafeous mixture; of methane with ethane and with butane have been reported by Buder.-I~olzer, Sage and Lacey.2 Brown1 predicted temperature drops for pressure drops from enthalpy-entropy calculations. Aside from this work there were no fundamental data found which would be applicable to natural gas mixtures of varying spe-

Jan 1, 1951

By Dwight H. Seely, Louis R. Records

A process for low-temperature dehydration of natural gas utilizing Joule-Thomson effect in expansion through a throttling orifice has been tested in a full-scale field installation. The results of these tests are presented in the form of performance curves from which the process may be easily evaluated. The effect of separation temperature on condensate recovery from the process is also shown. INTRODUCTION The transportation of natural gas from producing well to the consumer has always encountered the problem of hydrate prevention. This problem has become increasingly important in the past ten years due to the rapid increase in produced gas volumes, production pressures, transportation pressures and distance from producing wells to consumer. Natural gas, as normally produced from gas or gas-condensate wells, is saturated with water vapor at well-head conditions of temuerature and pressure. The solution of the hydrate problem require; but one basic process — dehydration of the gas to a water content which will result in a water dew-point below the minimum temperature to be encountered from the producing well to the point of consumption. Much of the recent development of gas and gas-condensate reserves in the Gulf Coast Area has been in locations which are accessible only by water. High well-head pressures, pipeline construction and maintenance costs and the desirability of final central gas-condensate separation facilities have stimulated the development of dehydration equipment which can be installed at each well and which will permit hydrate-free transportation of both gas and condensate in the same line to central facilities. There are four types of natural gas dehydration processes now used: 1. Adsorptive processes. 2. Absorptive processes. 3. Chemical reaction processes. 4. Refrigeration processes. The first three of these processes are indirect in that they require use of adsorbents, absorbents or reactive chemicals. These materials require regeneration and part of the total gas stream is consumed in the regenerative process. Indirect processes have a wide range of flexibility as defined by allowable operating pressure and temperature, but most are not easily adapted to automatic operation. The refrigeration process described in this paper was designed for installation at the producing well-head. It requires no regenerative cycle and with normal well-head temperatures no external source of heat. The flexibility of this process is limited only by the pressure drop which may be allowed between well-head and transportation line. THEORY There are three basic physical concepts involved in the low temperature dehydration process. These are: 1. Formation of hydrocarbon hydrates. 2. Joule-Thompson effect resulting from the expansion of gaseous mixtures through a throttling orifice. 3. The equilibrium composition characteristics of water vapor and gaseous hydrocarbon mixture.. The chemical composition and physical structure of hydrate; have been described by several investigators.3,4,5,10 Specific conditions of temperature, pressure and composition as well as the requirements for turbulence and presence of free water necessary for hydrate formation have been described by Katz.6 Natural gas hydrates, as they are found in plugged gas pipe lines, have the appearance of packed snow. The mass of these hydrates has low continuous porosity and permeability. Joule-Thomson effect. or the reduction in temperature which occurs when natural gas is throttled throusll a restrictive orifice, is the basic phenomenon which permits efficient use of refrigeration for the purpose of dehydrating natural gas. Joule-Thomson coefficients for gafeous mixture; of methane with ethane and with butane have been reported by Buder.-I~olzer, Sage and Lacey.2 Brown1 predicted temperature drops for pressure drops from enthalpy-entropy calculations. Aside from this work there were no fundamental data found which would be applicable to natural gas mixtures of varying spe-

Jan 1, 1951

By G. P. Bowman, D. F. Howard, R. K. Saxer, J. R. Myers

This study was undertaken to redetermine the phase diagram of the lead molybdate-bismuth molyb-date salt system. A portion of this diagram was originally determined by Zambonini in 1920, and more recently by Beale. Thermal analysis and X-ray methods were used to define this system. The diagram was found to be a simple eutectic type with an eutectic at 11 mol pet lead molybdate and 634OC. A maximum solid solubility of 6 mol pet was found at the lead molybdate end of the diagram. Solid solubility at the bismuth molybdate end of' the diagram appeared to be quite limited and possibly nonexistent. These results generally agree with those of Beale, but differ significantly from those of Zambonini. MOLTEN salt systems have been vigorously investigated since World War 11. Much of this work has been performed as pure research; however, consideration has recently been given to their possible use as coolants in nuclear reactors. Because of this application and other potential applications, it was decided to reinvestigate the lead molybdate-bismuth molybdate phase diagram. This diagram was originally determined by Professor F. Zambonini of the University of Turin in 1920.' In 1961, a portion of this diagram was redetermined by Beale.2 With the quality equipment and high-purity materials available today, it was expected that discrepancies between the results of this present investigation and Zambonini's work would be obtained. This investigation was conducted in two parts. First, the general shape of the phase diagram was determined by cooling-curve analysis. Next, the primary solid-solution phase at the lead molybdate end of the diagram was investigated by means of X-ray diffraction techniques. EXPERIMENTAL PROCEDURE High-purity lead molybdate, assaying 99.993 pet, and high-purity bismuth molybdate, assaying 99.989 pet, were employed during this investigation.* The results of a spectrographic analysis of the two salts are presented in Table I. Twenty-two experimental compositions were prepared for cooling-curve analysis. Compositions selected are presented in Table 11. Several randomly selected samples were analyzed chemically to check that the compositions of the prepared specimens were within the limit of

Jan 1, 1964

By P. Schwarzkopf, J. H. Brophy

A modification of the Mendenhall wedge blackbody1 has been used to determine solidus temperatures and to anneal alloys in the tantalum-rhenium binary system. The technique has proven to be simple and accurate with modest power requirements. For temperatures up to 2800° C a piece of 10-mil tantalum sheet was folded double and formed as shown in Fig. 1. The middle of the resulting ribbon filament was a cylindrical-shaped crucible with less than a 1/8-in. opening. After inserting a specimen in the cavity, the filament was clamped between molybdenum electrodes in a high vacuum chamber. A representative filament 2 in. long and % in. deep was heated to 2800°C with a current of 700 amp at 4 v. The specimen temperature was determined by sighting into the cavity with a Leeds and Northrup optical pyrometer. The twisted filament shape was necessary to avoid serious geometric changes during thermal expansion. For temperatures between 2800" and 3000°C a 4-mil tungsten filament was employed. To facilitate fabrication it was warm-folded, and a twisted segment of 10-mil tantalum was used to support one end to absorb thermal expansion. This element assembly required about 700 amp at 10 v to reach 3000°C. Two geometric modifications of the filament were helpful for solidus temperature determinations. A shallow chamber, with depth to opening ratio of 3 to 1, permitted direct observation of the specimen through the optical pyrometer. The fact that the specimen was visible permitted the melting point to be determined when sharp features on the specimen surface became rounded; it also indicated that blackbody conditions did not prevail. By standardizing against the melting point of molybdenum, the observed melting temperature was corrected by the following form of Wien's Law: in which T is the true temperature, To is the observed temperature, and K is a constant characteristic of the filament geometry and determined experimentally for the molybdenum standard. The resulting corrected melting point for each alloy served as a reference temperature for the second more precise filament geometry. With a 6 to 1 depth to opening ratio, the specimen was indistinguishable from the filament interior, indicating good blackbody conditions. Using this technique, a series of specimens was isothermally treated at temperatures above and below the corrected direct reading. Incipient melting was detected by visual or micrographic examination of the specimen after cooling. This procedure was checked with specimens of pure chromium, molybdenum, and tantalum. Table I represents the values obtained, together with the solidus temperatures in the tantalum-rhenium binary system determined by the same technique. The alloy specimens were approximately 1/8 in. in diam. They were pieces of 10-g buttons melted four times in a nonconsumable tungsten electrode arc furnace on a water cooled copper hearth in 2/3 atmos of titanium gettered helium. Several sources of error are possible in such temperature measurements. Within the accuracy of the pyrometer no gradients were detectable near the specimen, and element distortion was virtually eliminated by twisting the tantalum. Compensation was made for the 1/8-in. sight glass by inserting several identical thicknesses and extrapolating to zero thickness. As a result an additional 10°C correction was added to all observations in the temperature range of 2500" to 3000°C. The principal source of error was then in the operation of the

Jan 1, 1961

By S. S. Shen, M. J. Pool, P. J. Spencer, J. R. Guadagno

VERY few thermodynamic data are available for rare-earth alloys, partly because of the difficulties of obtaining the metals in sufficiently pure form and also because of their comparative scarcity up to the present time. The rare earths form a very interesting series in the periodic table in view of the progressive filling of their 4f subvalence electron shell and would be expected to provide useful information with regard to alloying characteristics of transition elements. It has been found in recent calorimetric investigations that the heats of solution of a number of the rare-earth metals in liquid tin are highly exothermic.1-4 Exceptionally strong bonding between rare-earth and tin atoms is clearly indicated in the liquid solutions. Continued thermodynamic studies of the behavior of rare earths in solution could thus contribute a great deal to present theoretical knowledge of alloying behavior and would yield an insight into bonding of a strength hitherto unencountered in liquid alloys. The determination of the heats of solution of the pure components in liquid tin is an essential preliminary to calorimetric work of this nature. Heats of solution of praseodymium, neodymium, and samarium in liquid tin at 750" ' and the heats of mixing of Pr-Nd solid solutions' have already been determined in this laboratory. The present investigations with lanthanum continue the study of rare-earth elements. Details of the construction and operation of the liquid metal solution calorimeter used in this work have been published previously by Pool and Peluso and no further description will be given here. The lanthanum used in heat of solution determinations was supplied by Lunex who quoted the purity as 99.9 pct. Their detailed analysis of the material is given in Table I. Samples of 0.0003 to 0.0005 g-atom were used for each run and great care was taken to remove all surface oxide prior to weighing. The samples were stored at all other times in a beaker of oil to prevent their otherwise rapid oxidation. The compounds LaSn (Cudu, L1P type structure) and La&, (structure not classified) were prepared from the appropriate quantities of the two pure components by arc melting under a purified argon atmosphere and once again great precautions were taken to avoid any subsequent oxidation of the specimens. Although no structural examination of the compounds was made, the consistency of thermodynarnic measurements carried out on twenty or so individual samples of each indicates that the compounds were in fact homogeneous, single phase alloys. Samples of the compounds consisting of 0.0003 to 0.002 moles were used in the calorimetric measurements. A solvent bath consisting of approximately 80 g of 99.9 pct pure Sn was used for each series of runs and its heat capacity was determined at regular intervals throughout the experiments using pure tin or tungsten calibration samples. Measurements were made of the heat of solution of lanthanum in liquid tin at 725", 750C, and 775°K and at compositions up to 2.21, 4.76, and 5.25 at. pct La at the three temperatures respectively. In every case, the heat of solution of lanthanum remained constant at its limiting value, within experimental limits, up to the highest lanthanum concentration investigated. Since no change in was observed, it was concluded that the liquid/liquid + LaSn, phase boundary had not been

Jan 1, 1969

By R. W. Armstrong, P. C. Jindal

WE should like to point out that Hu and cline.1 in their study of the recrystallization of titanium, have obtained data which appear very important for accurately determining the dependence of hardness on grain size for this material. It has been proposed2,3 that the macrohardness. H. of a poly crystalline material should depend on its average grain diameter, l. in accordance with the relationship: H =H0 + kHl-1/2 [1] where Ho and kH are experimental constants. This relationship follows from the hardness dependence on yield stress or flow stress4 and. thence. the Hall-Petch stress-grain size relations.5'6 Fig. 1 shows the Diamond Pyramid Hardness. Dph. values vs the reciprocal square root of the average diameter of the recrystallized grains, taken from the titanium data reported by Hu and Cline. The data in this figure give a linear relationship for the hardness over a wider range of grain diameters than anyone has previously measured. The data are not linear, for example. on an I-1 or l-1/3 scale. At the very large grain sizes the data are in reasonable agreement with measurements earlier reported by Holden, Ogden, and Jaffee.7 For the grain sizes smaller than 1 µ, which correspond in Fig. 1 to hardness values greater than 150, the material was reported as not being completely recrystallized and, therefore, these data appear less meaningful as far as the hardness dependence on grain size is concerned. However. it has been suggested by other investigators that deformed materials exhibit strengthening due to an effective grain size refinement even in the unrecrys-tallized condition.8-10 Also. Hu and Cline have shown that a change in texture occurs for titanium during the recrystallization process and. especially. following it. The influence of this texture change on the hardness-grain size relation would be expected to be less than that reflected in the unidirectional stress-strain behavior, even for an hcp material. because of the actual combined stress system which applies for the hardness test. For, at least, certain combined stresses, average values of the orientation factors should still occur in the stress-grain size analysis of a material exhibiting a preferred orientation.' We previously suggested3 that the experimental constants. H0 and kH. from the Meyer hardness-grain size relation should be correlated with the Hall-Petch constants, uoy and ky.5,6 Our recent study" of the Hall-Petch relation and the hardness-grain size results which obtain for a number of polycrystalline materials shows that: The inequality [2] is explained by noting that the hardness should be correlated. perhaps, with the flow stress at some value of strain, as suggested by Dugdale,12 and. also, that the influence of strain on the Hall-Petch relation is to increase uo and not change k very much." Normally. Dph values and Brinell hardness values are nearly equivalent to each other and to the Meyer hardness number. For the case of titanium, then. the inequality [2] may be evaluated using the experimental values of ao = 8.0 kg per sq mm and ky = 1.3 kg per mm3/2 obtained from the experiment of Guard.6,13 Thus, (Ho/uo) = 12 and (kH/k3) = 1.3. This research has been supported at the University of Maryland through the Center of Materials Research by the Advanced Research Projects Agency of the U.S. Government.

Jan 1, 1969

By B. Lustman

IT has been known for a number of years that the addition of certain alkaline-earth and rare-earth metals to nickel-chromium base electric resistance alloys causes marked increase in their oxidation resistance as measured in an intermittent oxidation test similar to the ASTM—B 76-39 test. However, the mechanism whereby such additions confer protection is still unknown. On the basis of the experimental observation that the increase in life in intermittent tests of nickel-base alloys is proportional to the atomic radius of the added element, Hessen-bruchl has proposed that the added metal ions occupy holes in the oxide lattice which prevent diffusion of nickel ions in the oxide. Horn2 has postulated that the effect of such additions is to accelerate the rate of diffusion of chromium atoms in the metal and thus to favor the formation of Cr2O3 scales. Hickman and Gulbransen3 concluded from electron diffraction observation that the addition of the elements in question results in the formation of a barrier to the diffusion of nickel ions to the surface. In connection with some experiments conducted to develop a test for the resistance to oxidation of alloys in massive form under conditions of intermittent heating and cooling, some features of the oxidation of nickel-chromium base alloys were revealed which may serve to elucidate the mechanism of protection conferred by rare-earth and alkaline-earth elements. Specimens of cylindrical shape 0.360 in. diam x 0.37 in. long were placed in alumina thimbles and inserted into and withdrawn from a Globar-heated furnace operating at 2150°F at 7.5-min intervals. The weight of oxygen absorbed as well as the weight of oxide spalled were measured at intervals. With the particular experimental conditions used, the specimens in a 7.5-min cycle were at temperature for 2 min which corresponds to the heating time of the ASTM test. The weight changes of similar specimens under conditions of continuous heating in air at 2150°F were also measured. The specimens after oxidation were examined metal- lographically and samples of the spalled oxide collected for X-ray diffraction identification of the phases. The specimens used were from the same lot of material used by Hickman and Gulbransen3 and had the compositions shown in table 1. Included in table I are results of ASTM life tests on the materials in the form of wires. These materials, their composition and the ASTM life test data thereon were all supplied by F. E. Bash of the Driver-Harris Co. It may be noted that alloy 13246 of 80 pct nickel, 20 pct chromium nominal composition showed the shortest life in the ASTM test; alloy 12246 with the addition of small amounts of the elements zirconium, calcium, and aluminum, intermediate life; and alloy 12046 with the further addition of silicon, the longest life. In fig. 1 are shown the results of intermittent oxidation tests made on bulk specimens at 2150°F as well as continuous tests conducted at the same temperature. Duplicate tests were made on each specimen. The ordinate scale, inches of metal oxidized, was derived from the experimentally observed weight gain of oxygen by assuming the scale to be entirely Cr2O3. It may be noted that the metal-loss curves during intermittent oxidation show a constant or continuously increasing rate of weight

Jan 1, 1951

By D. O. Hobson, P. L. Rittenhouse

We have recently found that many lots of Zircaloy-2 and -4 tubing tested in tension deform to cross section shapes that are "polyhedral" rather than circular. The noncircular cross sections seem to result from a circumferential variation in plastic proper -ties and, therefore, in texture. We examined the diffracted X-ray intensity from (OOOl), {1010), {ll20}, and {1011} planes parallel to the tubing surface around the entire circumference. Tubing that deformed to a circular cross section showed <5 pct variation in diffraction intensity around the circumference from any of these planes. Greater intensity variations were found for all the tubing materials that developed non-circular cross sections during deformation. In each instance the number of intensity maxima and minima was consistent with the number of sides of the &apos;polyhedral" cross section. THE effects of crystallographic texture on the mechanical properties of zirconium, zirconium alloys, and other anisotropic hexagonal materials such as titanium and hafnium have been intensively studied. If the natural crystallographic anisotropy of these materials could be controlled by selected fabrication operations, a material could be produced with a texture, or preferred orientation, in which the maximum strength directions are in the stress directions of the structure. The permissible stress levels of the structure could then be increased. Rittenhouse and Pickle-simerl have shown that highly textured Zircaloy-2 plate can vary from 52,000 to 70,000 psi in tensile yield and from 62,700 to 122,000 psi in compressive yield strengths as a function of specimen orientation. Similar texture effects have been observed in Zircaloy tubing, whose mechanical properties differ depending upon whether the tubing has basal poles predominantly radial or tangential and upon the mode of testing. These same texture effects might be troublesome if the texture in the tubing is not uniform around the tube walls. This paper is concerned with the effects of nonuniform texture on the strain behavior of commercial Zircaloy tubing. BACKGROUND Previously, various lots of commercial Zircaloy tubing were tested under selected stress conditions as part of a program to determine the four quadrants of the yield locus. One of the testing procedures was uniaxial tension and it is the influence of texture variations on the tensile deformation behavior of the tubing that is of interest here. The effect of texture on the strain behavior in tubing is very apparent from a uni-axial tensile test.2 This behavior is illustrated schematically in Fig. 1 for three different tubing textures: 1) basal poles predominantly in the radial direction; 2) basal poles predominantly in the tangential direction, and 3) basal poles equally distributed between the radial and tangential directions. In the first example most of the grains are oriented for prism slip to operate to allow axial lengthening and diametral reduction of the tube. Reduction in wall thickness requires {1122} twinning, a more difficult operation than slip.* In the second example, the texture is such that *The singleCrystal analogy will be used quite often in this paper when strong texturesare being discussed. The textured material is assumed to react as if it were a single crystal aligned in the same orientation and under the same stress system as the predominant texture._____________________________________________ prism slip operates to give axial lengthening and wall thinning. Diametral reduction requires twinning and again should be more difficult to accomplish. A specimen with basal poles equally distributed between the radial and tangential directions should exhibit about equal diametral and wall strains.* Table I shows the *Diametral strain is accomplished by a combination of circumferential and longitudinal strains. But, for the purposes of this paper, it will be considered as a strain causing a change in the length of a specified diameter.__________ strain behavior of two lots of tubing with different textures. The first tube has a texture with basal poles equally distributed between the radial and the tangential directions. The ratio of true thickness strain to true diametral strain is almost unity. The second tube has a predominantly radial basal pole texture and it is apparent that most of the total strain has occurred by diameter reduction, just as one would predict. There is over three times as much diametral strain as thickness strain. RESULTS We found that specimens from certain lots of commercially fabricated tubing did not retain round cross sections during uniaxial testing. Instead, the speci-

Jan 1, 1970

By Tibor Stefansky, John E. Dorn

MOTT and Nabarro1-5 were first to illustrate the importance of the flexibility of dislocations in accounting for the strengthening that metals undergo due to the presence of internal-strain centers. Such strain-centers might arise from a number of causes such as radiation damage, the presence of semicoherent and coherent precipitates and clusters, as well as individually dispersed interstitial and misfit substitutional solute atoms. Each strain-center induces positive and negative shear stress fields on the slip planes of the surrounding alloy matrix. In order to effect plastic deformation, therefore, the alloy must be subjected to sufficiently high applied shear stresses to push dislocations past all such internal stress fields. If dislocations were inflexible and moved as rigid lines, they would be equally pushed and pulled by internal stress fields. At this extreme the strengthening would be vanishingly small. Dislocations, however, are not rigid; they are flexible and extensible. They wiggle between positive and negative strain-centers, thus increasing their line energy at the expense of their interaction energy with strain-centers. cottrel16 and Friedel7,8 have independently presented lucid reviews of the significance of the Mott-Nabarro dislocation-flexibility concept to the strain-center strengthening of alloys. Their analyses however were only semi-quantitative. There is evidence in the recent literature of renewed interest in a more rigorous analysis of flexibility. Thus, Gleiter9 and Gerald" have shown that the calculated strain-energy interaction between a dislocation and the stress fields of coherent precipitates can be seriously in error if the flexibility of the dislocation is not taken into account. This report will be concerned with a more detailed analysis of the problem based on the following approximations: 1) Although many types of strain-centers exist, the following analysis will be limited to the case of solute-atom strain-centers in fcc substitutional alloys. 2) To facilitate the analysis by avoiding statistical considerations, the strain-Centers are assumed to be in regular arrays on the slip plane. Although the quantitative results are somewhat dependent on the type of array that is assumed, the qualitative trends are similar for various arrays that were studied. 3) An adjustment of the results from those for square arrays to those for the more realistic case of a random distribution of strain-centers is accomplished by adopting the interesting statistical theory first introduced by Kochs,11,12 elaborated on by Dorn, Guyot, and stefansky,13 and analyzed by Foreman and Makin14 in their computerized experiments. 4) For simplicity the dislocation lines are taken to wiggle about their edge orientation and no correction is applied to their line energy for deviations from edge configurations or for the elastic interaction between segments of the now curved dislocation. It will be shown that for extremely low concentrations of atomic strain-centers the strengthening increases with the square root of their concentration. For slightly higher concentrations the strengthening rate becomes less rapid. At a critical concentration a maximum strength is obtained and a decrease in the strengthening takes place as the concentration of solute atoms is further increased. These trends are a direct consequence of dislocation flexibility. They arise from changes in the amplitude of the waviness of the dislocation line at the yield stress with solute atom concentration. Despite the simplifying assumptions that were made, the results agree qualitatively with appropriate experimental data. I) STRESS FIELDS ON SLIP PLANES Internal stresses are introduced in a lattice whenever a host atom of radius ro is replaced by another that has a different atomic radius. According to the classical theory of linear elasticity,15 the stress field about a solute atom at the origin of a spherical coordinate system is given by arr=-4G€(?_0)3 ffflfl ="W =2G€{t) f°rr^ro(l+e) UJ where G is the shear modulus of elasticity and Y, = ro(l + E) is the radius in situ, of the substituted atom. As shown by ~shelb~,&apos;~ this approximation assumes that the bulk modulus of elasticity of the substituted atom is identical with that of the host species. ~abarro&apos;~ suggested that the strain E can be deduced

Jan 1, 1970

HUBERT INGERSOLL ELLIS Hubert Ingersoll Ellis, who met accidental death on Jan. 6, 1919, in eastern Washington, had already advanced far in the profession of mining engineering and gave promise of a brilliant future. He was born on the Washington coast in June, 1889, and had his preparatory schooling at Menlo, Wash. In 1905; he entered the College of Mines of the University of Washington, and at once made a high record of scholarship. After completing 3 years of his technical course, he went to the interior of Alaska, where he spent 4 years in mining. During this time he was field correspondent for technical-magazines and wrote several important articles. In 1915, Ellis completed his senior year in the College of Mines; his graduation thesis was a comprehensive paper on mining methods at Fairbanks, Alaska, which was published as a series of articles in the Engineering and Mining Journal. On July 14, 1915, he entered the employ of the Bunker Hill & Sullivan Mining & Concentrating Co., Kellogg, Ida., as an underground miner, and was soon promoted to the position of operative on experimental metallurgy and later chemist in the same work. Later, he did exhaustive work on flotation with particular attention to the use of various addition agents. For the past 212 years, his work was largely in the field, examining mining prospects and directing work of investigation, during which time, while located at Sumter Valley, Ore., in 1916, he was elected to membership in the American Institute of Mining and Metallurgical Engineers. During the same year, he was married to Miss Grace Wells, of Arkadelphia, Ark., and besides his widow leaves a young son. In Hubert I. Ellis, there was found the rare combination of executive, administrative, and business ability, together with a temperament exceptionally well adapted and trained for research work and for the careful and exhaustive examination of engineering problems, both practical, and academic. These qualities were in addition to a splendid physique and a personality that made him highly successful in the handling of sub-ordinates and in his contact with his associates and the public.

Jan 4, 1919