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By P. H. Dudley

I have taken the liberty of calling the researches herein mentioned industrial, to distinguish them from those strictly scientific, where every known appliance is used to insure accuracy in determining principles. The industrial researches are made to ascertain wherein we have failed to embody, in practice, the principles which have been fully demonstrated by the more purely scientific investigations. So far the researches have been mostly confined to the conditions of combustion as used in locomotive furnaces, although we have examined, to some extent, furnaces under marine and stationary boilers. The products of complete combustion are gases, and, knowing what we should have, it is at once shown by analyzing the products whether the desired reactions are taking place. In spite of imperfect furnaces, lack of system in the arrangement of grate-bars and exhaust nozzles, the results are not altogether vitiated, because the analyses are not closer than one-tenth of one per cent., as under the present conditions it is hardly possible to collect gas exactly under the same conditions at different times. All of 'our industrial operations have developed in the past few years so rapidly, nearly all of them paying, that,, until within the past three years, comparatively little attention has been given to their economy outside of the profession. Great corporations have not asked and considered the question in earnest, can we utilize our heat so as to produce the same effect at less cost? The applications of heat are so extensive, entering into every branch of industry, the principal power used to carry on metallurgical processes, to conduct transportation, that its econonlical generation becomes of universal importance; in fact, its economical generation and application is the leading industrial question of the day. It is stated by those who have given the subject much attention, that in our best steam-engines not over 10 per cent of the theoretical value of the fuel is utilized, and upon locomotives it is far less, probably not exceeding under the most favorable circumstances 5 or 6 per cent. In recent experiments made with the dynagraph, in drawing trains upon the Lake Shore and Michigan Southern Railway from Cleveland to Erie, 941/2 miles, we found the force required to draw a stock train of 709 tons to be 2,498,396,320 footpounds, exclusive of the force to move the locomotive itself. We

By Sanai Nakabe

Japanese wartime economy demanded domestic cobalt production. This paper describes a process operated for two years at the Besshi mine and smelter on extremely low grade (0.1 pct Co) pyrite concentrates obtained from copper ore. 'The steps in the process were roasting, leaching, precipitation, reduction fusion to crude cobalt, and finally refining by electrolysis to 99+ pct. COBALT ore deposits in Japan are all small and of poor grade. In the past, a small amount of cobalt has been produced from the best portions of a few of these deposits, and very little production is expected in the future. In addition to these lean cobalt ores, cobalt is present in the cupriferous pyrite which is fairly abundant although of low grade, as is shown in Table I. Considerable cobalt is expected from these deposits because of their extent. Cobalt cannot be exclusively recovered economically from ore of this type; however, if means could be devised to recover it as a byproduct of copper production, a fairly large production at reasonable cost could be expected from Japanese sources. It was along this line that the research work was done. Selection of Suitable Process The process for extracting cobalt differs from ore to ore according to their composition. The difficulty in cobalt metallurgy arises from the fact that chemically cobalt resembles many such common metals as Mn, Fe, Ni, Cu, and Zn, associated with it in the ores. In the present case the most serious difficulties were: 1—Extremely low grade ore, 0.1 pct Co. 2—The large proportion of iron accompanying cobalt and its close similarity in chemical behavior. 3—The fairly large proportion of zinc and manganese and their chemical similarity to cobalt. The recovery of cobalt oxide as a byproduct of the hydrometallurgy of copper had been attempted in Japan but was stopped after a short period because it proved uneconomical. The literature disclosed no method for the recovery of cobalt from cobaltiferous copper pyrite and it was therefore necessary to devise a new process. The following basic principles were considered in selecting the process: 1—A major alteration in copper production methods should not be necessary. 2—The first step should be the extraction of cobalt leaving the large quantity of iron unaffected. For this purpose wet metallurgy would be preferred.

Jan 1, 1952

By Frederick Laist, Howard Aldrich

The object of the construction and operation of the 80-ton leaching plant was to test out the leaching of sand tailings on a large scale and, if possible, determine a definite method of operation, and the best construction for the larger unit which is now being built. It was also of importance to obtain some practical data as regards cost items. The 80-ton plant was not expected to be a commercial success. A leaching process on such low-grade material necessitates the treatment of a very large tonnage. Such a cost item as labor, for instance, is entirely out of proportion in such a small plant. The amounts of acid, salt, scrap iron, and fuel for roasting, however, are the same per ton in an 80-ton plant as in a 2,000-ton plant. These costs were definitely established. Also the percentages of extraction and grade of tailings were definitely determined for a large-sized unit. Following will be found the description of the plant, the method of operation and the- results obtained. A general view of the plant is given in Fig. 1. The bins consisted of one coal bin with a capacity of 30 tons, one salt bin with a capacity of 20 tons, and a "mill tailings" or feed bin which held 70 tons. The coal and salt bins were placed with their floor level even with the firing floor of the roasting furnace. The feed bin, to give it greater capacity, discharged about 12 ft. below this point, to a 12-in. conveyor belt, which in turn discharged into a pug mill. This fed another conveyor belt, which discharged into the top hearth of the furnace. The furnace was an ordinary six-hearth MacDougall roaster, 20 ft. in diameter. It was equipped with two fire boxes, on opposite sides, the flames entering on the third hearth. An induced draft was obtained with a Buffalo blower, worked as an exhaust fan. Just above the top hearth was an annular flue around the whole circumference of the furnace. Slots at intervals of about 18 in. led from this flue down into the top hearth. The slots were 2 in. wide by 6 in. long. This annular flue proved rather unsatisfactory, as it tended to fill up with flue dust and choke the dots, thus cutting down the draft. The volume of gas through

Jan 1, 1915

The primary purpose of the Institute is to advance the technologic and engineering arts embraced by it through interchange of knowledge. This can best be clone by the presentation and discussion of technical papers by its members. Short practical papers are especially welcome. An author should always satisfy himself that his material is of a quality that will he a credit to him and to the Institute. The preparation of a good paper frequently leads to a reorientation of the author's thoughts, and publication contributes much to the professional standing of the author. Members are urged to submit papers presenting the results of their work. Attention to the following suggestions will greatly further the prompt and efficient handling of manuscripts. 1. SUBJECTS: The subject must be within the field of the Institute. Original work, the results of field, plant, laboratory or theoretical investigations, new views on old but important problems and occasionally reviews of timely and important subjects of wide interest to our members may constitute the basis of a paper. The mere fact that the work is original does not necessarily justify publication: it must be of a substantial nature, of value to a reasonable number of our members and worthy of permanent record. It is seldom desirable to subdivide the results of a single research for publication in a variety of journals. Previous publication is usually a bar to acceptance. If any part of your paper has been published elsewhere and you regard repetition as absolutely necessary please so state in your covering letter. 2. CONSTRUCTION: Papers should be clearly and concisely written in good English. Care in this regard ensures wider reading and the saving in space permits the Institute to publish more papers. It is the experience of the Papers and Publications Committee that most papers can he improved by condensation. "Readers" who are asked to recommend acceptance or nonacceptance put particular emphasis on the length of the paper and the elimination of unnecessary or any extraneous material. The terminology and units employed should be those current in the particular field. An examination of Institute publications will afford useful guidance in such matters. Webster's New International Dictionary, 1935 edition, is the Institute's authority for spelling and style. Various abbreviations are used habitually; for instance, lb., pound; bbl., barrel or barrels; ft., foot or feet; hr., hour or hours; in., inch or inches; Fig. 1 but Figs. 2 and 3.

Jan 1, 1946

By David A. Keys

The actual procedure in estimating depth of overburden from magnetic observations made on the surface will vary with the form of the deposit and any theoretical discussion will apply only so far as the form of the deposit conforms to the mathematical premises on which the theory is based. Since the shapes of natural deposits in the field cannot be expressed rigorously in mathematical form, the best that can be done is to assume some simple form and deduce results. Fortunately many small variations in form produce only slight changes in the estimated depth of overburden, therefore the methods have a definite practical value. For the theoretical treatment, magnetic ore deposits may be divided roughly into three classes, depending upon whether the magnetic anomalies may be considered to arise from (1) a single magnetic pole, (2) a dike or (3) a magnetic doublet. Particular cases, falling under one or other of these classes, have been discussed by different authors.1"4 In general, it may be stated that when the magnetic effects as measured on the surface are due only to one pole of the body, the other pole being so remote that its effect may be neglected, the resultant anomaly F at any point will vary as the inverse square of the distance r of the point from the pole, which may be expressed mathematically by F = k/r2, where k is a constant. When the deposit occurs in the form of a long, thin dike, the resultant anomaly will be of the form F = k'/r and when the deposit is in the shape of a lens, so that both poles have an appreciable effect on the surface, the result will be similar to that caused by a magnetic doublet, and the form will be F = k'/r3. The particular class under which a deposit falls may be deduced from the results of the magnetic survey. The second class is readily found, but there may be difficulty in deciding between the first and third. Isody-namic contours of both the vertical and horizontal anomalies will often be a good guide in making a correct decision. The correctness of the theoretical calculations may be checked in two ways. The first is to make laboratory models of various known shapes and pole distributions, to calculate the anomalies to be expected

Jan 1, 1940

By David A. Keys

The actual procedure in estimating depth of overburden from magnetic observations made on the surface will vary with the form of the deposit and any theoretical discussion will apply only so far as the form of the deposit conforms to the mathematical premises on which the theory is based. Since the shapes of natural deposits in the field cannot be expressed rigorously in mathematical form, the best that can be done is to assume some simple form and deduce results. Fortunately many small variations in form produce only slight changes in the estimated depth of overburden, therefore the methods have a definite practical value. For the theoretical treatment, magnetic ore deposits may be divided roughly into three classes, depending upon whether the magnetic anomalies may be considered to arise from (1) a single magnetic pole, (2) a dike or (3) a magnetic doublet. Particular cases, falling under one or other of these classes, have been discussed by different authors.1"4 In general, it may be stated that when the magnetic effects as measured on the surface are due only to one pole of the body, the other pole being so remote that its effect may be neglected, the resultant anomaly F at any point will vary as the inverse square of the distance r of the point from the pole, which may be expressed mathematically by F = k/r2, where k is a constant. When the deposit occurs in the form of a long, thin dike, the resultant anomaly will be of the form F = k'/r and when the deposit is in the shape of a lens, so that both poles have an appreciable effect on the surface, the result will be similar to that caused by a magnetic doublet, and the form will be F = k'/r3. The particular class under which a deposit falls may be deduced from the results of the magnetic survey. The second class is readily found, but there may be difficulty in deciding between the first and third. Isody-namic contours of both the vertical and horizontal anomalies will often be a good guide in making a correct decision. The correctness of the theoretical calculations may be checked in two ways. The first is to make laboratory models of various known shapes and pole distributions, to calculate the anomalies to be expected

Jan 1, 1940

By W. D. Robertson

A considerable quantity of experimental data is available on the effect of time, temperature, work-hardening and composition on the mechanical properties and corrosion resistance of aluminum alloys. There is, however, little unity of purpose or generality in most of the studies and, because the number of variables is large, the results often are not applicable to the problems that arise in practice. Furthermore, the customary expression of the effect of different variables as separate curves or as three-dimensional diagrams with time, temperature and the dependent variables as coordinates, renders the task of selecting the optimum time and temperature of precipitation treatment, with respect to their simultaneous but unequal effect on the various properties, exceedingly difficult. The introduction of precipitation treatments to raise the yield strength of 24S-type alloys has created a need for a method of correlating and summarizing the effect of time and temperature on the mechanical properties and susceptibility to intercrystalline corrosion. Correlation is particularly desirable because the choice of time and temperature is of necessity a compromise to achieve the best possible combination of properties, and the optimum conditions cannot be accurately specified unless the data are in a form in which the alternatives can be readily compared. Therefore, the work described here was undertaken to find a common relationship that would be capable of expressing the effect of precipitation time and temperature on the various properties and by means of which the relative effects could be correlated and their interpretation facilitated. REVIEW OF PREVIOUS WORK In connection with an investigation of the interrelation of age-hardening and creep performance of nickel-silicon-copper alloys, Jenkins and Bucknall1 demonstrated that the time required to attain maximum hardness and tensile strength could be expressed by a relationship of the form: t = K. 10m/T (I) where t is the time in hours and T the temperature of aging, expressed in degrees absolute, and m and K are constants. They also pointed out that this expression is analogous to that which describes the change of the diffusion coefficient D with temperature; namely, D = Ae-Q/RT (2) Later, Cohen used this relationship in studies of the mechanism of age-hardening of a silver- rich copper alloy2 and of duralumin. 3

Jan 1, 1945

By T. T. Field, M. Gell

MUCH has been learned about plastic deformation behavior in crystals through the use of dislocation and slip band etchants. Slip in nickel and nickel-base alloys has previously been revealed by various etching techniques.l-5 The techniques for nickel-base super-alloys4,5 were successful only in the Udimet 700 composition in specific heat-treated conditions. The objective of this work was to develop a more generally applicable slip-band etching procedure. The nominal compositions of the alloys used in this study are listed in Table I. The low carbon Mar-M2OO alloy referred to in the text is the same as listed in Table I with the exception that the carbon content is less than 100 ppm. Mar-M200 and Udimet 700 were solutionized at 2250" and 2150°F, respectively. The aging treatment for both cast alloys was 32 hr at 1600°F and for wrought Udimet 700 was 4 hr at 1975"F, 24 hr at 1550°F, and 16 hr at 1400°F. The new slip-band etching technique consists of a chemical etch followed by a short electropolish, Table 11. Fig. l(a) shows the best result obtained on an internal section of a plastically deformed single crystal of Mar-M2OO when using a conventional slip-band etching procedure which consists of electropolishing followed by etching. Ghostlike traces corresponding to planar slip bands are observed, but the contrast between the bands and the background is weak. Fig. l(b) shows the same field using the new slip-band etching technique. After the etching step of this technique, the same ghostlike traces of Fig. l(a) are observed, but the subsequent electropolishing accentuates the slip bands and the subgrain boundaries while the rest of the matrix is being polished. Longer electropolishing obliterates the slip bands. The new slip-band etching technique makes use of the etchants and electrolytes that are normally used for a given material. Because of this, it should be possible to slip-band etch other nickel-base superal-loys by using existing etchants and electrolytes for a material and following the procedures outlined in the "Comments" section of Table 11. All the illustrative examples given below show internal plastic deformation in single crystals of regular and low carbon Mar-M200 in the solutionized and

Jan 1, 1970

By William Kelly

I AM-glad to have the opportunity at this time to say that I consider it a very great honor to be elected President of the American Institute of Mining and Metallurgical Engineers. It fulfills the proudest hopes of my ambition. There is, ,however, one drawback to my personal gratification-a feeling of unworthiness to have my name placed on the list with former Presidents of the Institute, with the brilliant Raymond who guided our society for so many years, with the versatile and lovable James Douglas, my first employer and my friend, a most generous benefactor of our Institute, with the skilful Holley, who gave to the manufacture of steel in this country, its first great impulse, to mention only three of the accomplished men who have preceded me. I assume that the honor of my being elected President of the Institute is not merely a personal one but that it should be considered a tribute to the wonderful progress in the art of mining, both underground and in open pits, and in the beneficiation of native copper and iron ores, which have been shown in the Lake Superior District and also a recognition of our members there and elsewhere who are living at the mines and directing the operations, upon the success of which the whole mineral industry depends.

Jan 1, 1924

By V 7. 0 / 300 dpi

WHEN the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick -was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of all average sample of this quartz is: SiO2,, 96.7; Fe203, 0.3; Al203, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then clumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the. material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected

Jan 9, 1913

By C. E. Ells, A. Sawatzky

The effect of neutron irradiation on tensile properties of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy has been evaluated for integrated neutron fluxes up to 3 x 1020 n per sq cm (E > 1 Mev). Specimen temperature during irradiation was normally 300°C. The material was studied both in annealed and in quenched and aged conditions. When the alloy (fab-ricatedfrom sponge zirconium) is quenched from a temperature =40°C below the a + ß/ß transformation and aged 6 hr at 535oC, neutron irradiation up to the maximum studied has little effect 071 reduction in area, although there is a drop in uniform elongation and the yield strength is increased by = 25 pct. Conversely, irradiation of the alloy in an annealed condition can result in much greater changes in properties, with yield-strength increases of up to 200 pet. The dose dependence of irradiation hardening obeys the saturation equntion proposed by Makin and Minter to explain hardening in copper and nickel: Act = C[1 - exp(-Døt)/1/2 A rnodel is proposed to explain the effect of niobium content and metallurgical condition on irradiatiotz behavior. THE Zr-Nb alloys form a class of material susceptible to marked strengthening by quench and age heat treatment. With niobium concentrations as low as 2.5 wt pet, strengths can be developed which are double those of annealed zircaloy-2.1 Since the neutron-capture cross section of the Zr-2.5 wt pet Nb alloy is nearly identical to that of Zircaloy-2, significant gains in power-reactor neutron economy could be obtained by replacing stressed in-reactor components of Zircaloy-2 with the heat-treated Zr-Nb alloy. When the solution heat-treatment temperature is in the high (a + ß) phase, then the tensile properties of the quenched (and aged at 500°C) material have been shown to be relatively insensitive to neutron irradiation.1-3 Addition of small quantities of copper to the binary Zr-2.5 wt pet Nb alloy gives a useful reduction to the corrosion rate in air and carbon di- oxide,&apos; and a ternary alloy of composition Zr-2.5 wt pet Nb-0.5 wt pet Cu was chosen for one component in the Douglas Point Reactor. This application utilizes both the corrosion resistance to a moist air-carbon dioxide environment and the strength developed by a quench and age heat treatment. By suitable choice of solution heat treatment and aging temperatures, tensile properties of the ternary alloy can be made nearly identical to those considered as optimum for the binary alloy. One effect of the copper addition, however, is to give marked changes in the aging kinetics of the alloy.&apos; For this reason, it appeared that neutron irradiation might promote overaging in the ternary alloy, particularly at the elevated service temperature (=300°C). This paper describes the effect of neutron irradiation on the tensile behavior of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy in several metallurgical conditions pertinent to its use as a reactor material. The metallurgical conditions included those for which aging occurs in the unirradiated material, and fully annealed conditions for which a higher degree of thermal stability could be expected. 1) EXPERIMENTAL Two batches of alloy were used, both made from sponge zirconium. The fabricator&apos;s analysis of principle constituents showed no significant difference between the two batches, Table I. The rod material was rolled to 1.5 in. diam, and then swaged to final sizes of 0.5 to 0.375 in. diam at nominal temperatures of 785" and 625°C for the AM and AS batches, respectively. Subsequent hydrogen analyses at CRNL confirmed that the hydrogen concentration of the as-received rod was indeed <20 ppm. However, it was found that the (a + ß)/ß transus for the AM material was approximately 25°C lower than that of the AS material, indicating rather more difference in oxygen concentration than given in Table I. Except for a small difference in yield-point behavior, the tensile prop-

Jan 1, 1965

By G. H. Kesler, J. E. Oberele, C. E. Dryden, J. H. Oxley

Heat-transfer rates were measured in a model of a multifilament vapor-deposition bulb fo the preparation of high-purzty metals. Local transfer coefficients for heat transfer frow the filaments to the circuates process stream were determined as a functiol of gas flow rates and bulb, inlet, and filament, geowzetvies. These results a-e then convertted to n mass-t7,ansfer basis to provide a method of correlating vapor-deposition rates and to predict the performance of commercial urzits. The firm1 cor?,elating equation for mass transfer was found to be- wheve k, is the mass-transfer coefficient; D, is bze gas difficsivity : P is the system pressure; R is the gas constant; T is the gas temperature; Df, DB, and Di ave tlze diameters of the filament, bulb, and inlet, respectively; k is the gas conductivity; C, is the specific heat of the gas, M is the wzolecular zleight of the gas; Npr . N,,, NRe a7&apos;e the Prandtl, Schmidt, and Reynolds numbem of the system, respectively; LB is the height of the bulb; and SB and Sf are the total suyiace area of the bulb and filaments, respectively. ONE of the more conventional methods of preparing very high-purity metals is the vapor deposition of the metal upon heated filaments. The reactions which can be employed in such a process generally fall into two classes: 1) Pyrolysis of a volatile metal compound. Generally because of their instabilities, metal iodides are used; however, other metal halides and hydrides have been employed. These processes are frequently carried out under vacuum conditions, and the filaments are maintained at high temperatures. 2) Hydrogen reduction of a volatile metal compound. A metal chloride is normally the preferred feed for these processes, but other halides are sometimes used under special conditions. These hydro- gen-reduction processes are usually operated at atmospheric pressure. Many of the current processes for the production of semiconductor materials are actually vapor-deposition processes. However, the vapor-deposition process itself is relatively old, and almost all metals can be prepared in a state of very high purity by the use of vapor-deposition techniques. Loonam has recently given an excellent review of the iodide process for metal deposition,&apos; and Owen has started some detailed studies with a carbonyl system.&apos; A more general treatment of all vapor-deposition processes has been outlined by Powell, Campbell, and Gonser.3 Despite the fact that vapor-deposition techniques have been employed since 1890, there is a surprising lack of fundamental information regarding the transport characteristics of even the simplest deposition system, the heated filament. The purpose of the investigation described in this paper was to extend some of the earlier data obtained at Battelle to predict deposition rates and the uniformity of deposition in large-diameter, multifilament deposition bulbs under forced convection conditions.4&apos;5 A number of other investigators have already presented a simplified treatment of the deposition process under non-flow conditions, i.e., pure diffusion.6"9 To obtain information on the transport characteristics of a deposition bulb, a model of a typical plant deposition unit was constructed, and local heat-transfer coefficients from the filaments to a circulating air stream were determined under various conditions of air-flow rates and bulb, inlet, and filament geometries. These results were then converted to a mass-transfer basis, and consequently provided a method to correlate experimental vapor-deposition rates and to design commercial deposition units. EXPERIMENTAL WORK Description of Model. The apparatus which was used in this work was a scaled model of one type of deposition bulb. It was constructed of Lucite and was easily altered to give several combinations of diameter of bulb liner, inlet size and location, number of filaments, and outlet geometry. The model is shown in Figs. 1 and 2. The bulb shell was made octagonal for convenience in construction and observation, and the bulb liners were cylindrical. Air, introduced through one of several different jet inlets, was used as the test fluid in these model studies. Filaments for deposition of metal were simulated by metal rods 1/4-in. in diam. Two of the rods could be heated by passing electrical current through them ¦ while the remaining rods could not be heated. This procedure minimized the amount of heat which was

Jan 1, 1962

By Rex B. McLellan

A simple model for dilute interslitial solid solutions is set up which enables a solubility equation for the equilibrium between the solid solution and the gaseous solute to be deduced. This solubility equation is used to estimate the partial thermody -namic functions of Ag-O and Fe-N dilute interstitial solid solutions from the measured equilibrium between these solutions and the gas phase. It is shown that the partial excess entropy of the solute atom in solution is a vibrational entropy which is due Principally to the oscillation of the interstitial atom and does not arise from electronic or elastic interaction between the solute atoms and solvent matrix. In this work measurements of the equilibrium between dilute solid interstitial solutions and a gaseous phase are used to deduce the important thermody-namic functions of the solid solution with the aid of a theoretical solubility equation formulated from a knowledge of the thermodynamic functions of the gas and a simple model for the solid solution. The quantity of principal interest which is deduced from the equilibrium data is the change in vibrational entropy occurring when a solute atom (u) is placed in an interstial site in the solvent (u) lattice. This paper forms part of a more general study in which the properties of condensed phases are deduced from measurements of the equilibrium between the condensed phase and a gas. Previous investigations have dealt with the equilibrium between krypton and liquid metals,&apos; a pure metal and its vapor,&apos; and dilute substitutional alloys and the vapor,3 and the subject has been popularly reviewed by McLellan.4 In the latter investigation3 the vapor pressures of very dilute Cu-Ag and Cu-Au alloys were measured with a Knudsen cell technique over a large range of temperatures and the analysis of the vapor-pressure data showed that the relative partial excess entropies were large and positive [ds= -Sudk = 30 for Au-Ag alloys and 150 for Cu-Au alloys; these values should be compared to unity, the value assumed for these exponentials in the quasi-chemical theory of solutions]. For many interstitial solutions experimental data is available for the equilibrium between the solution and a gaseous phase, and this can be used to deduce the vibrational entropies of the solute atoms in solution. The general method employed is to calculate the chemical potential of the solute atoms in the gas and equate this to pi, the chemical potential of solute atoms in the solid, which is deduced from a simple model set up for the dilute interstitial solution (in which the solute atoms act as bound oscillators in interstitial sites). This enables a theoretical solubility equation to be set up. In the case of Ag-O and Fe-N solid solutions the solubility c, is found to vary with temperature according to a relation of the type, where PU2 is the pressure of the O2 or Np molecules. Essentially, the theoretical solubility equation enables the parameter A(T), which gives the vibration entropy, and the parameter AH, which gives the energy of solution of a solute atom, to be estimated from the measured variation of solubility with temperature. The solutions treated are dilute enough to enable solute-solute interactions to be neglected so that the partial energy and excess entropy of solution E, and GS are not functions of composition and the configurational entropy is that of a random solution. Large positive values have been found for sxSu this quantity has not been given sufficient consideration in recent work on interstitial solutions and it is felt that the partial thermodynamic quantities of very dilute solutions should be understood before the thermodynamics of concentrated solutions can be fully appreciated. EXPERIMENTAL DATA 1) The Silver-Oxygen System. The measurements of Steacie and Johnson,= using silver foils, indicate that there is a pronounced minimum in the solubility vs temperature curve for O-Ag solutions. Eichenauer and Miiller6 have recently redetermined the solubility of oxygen in silver using a method developed in the investigation of metal-hydrogen systems.7 The solubility determinations were carried out on compact specimens of differing shapes and sizes and the results indicate a much lower solubility than was obtained by Steacie and Johnson with no minimum at 400°C. Subsidiary experiments showed that the erroneous results of Steacie and

Jan 1, 1964

By R. R. Vandervoort, W. L. Barmore

Tensile creep experiments were conducted on high-purity, poly cvystalline rhenium from 1500" to 2300°C at stresses from 1500 to I0,OOO psi in a vacuum of 10-a torr. The apparent activation energy for creep was 60 kcal per mole, and the steady-state creep rate varied directly with stress to the 3.4 power. Dislocation substructure that developed during creep was studied by transmission electron microscopy. Possible rate-controlling deformation mechanisms are discussed. The creep behavior of most metals at elevated temperature can be represented by the following equation:&apos;&apos;&apos; t = Cf(s)(^)(s/E)nD [1] where i = steady-state creep rate, C = constant, f(s) = a function involving microstructure, s = applied stress, E = the average elastic modulus at test temperature, n = constant, D = diffusion coefficient According to this well-established relationship, metals with higher elastic moduli and lower diffusion coefficients should have greater creep resistance at the same stress and temperature and equivalent mi-crostructures. While no diffusion data are available, the diffusivity of rhenium should be less than that for most other refractory metals because of its high melting point and hcp crystal structure. The Sherby-Simnad relation for calculating atomic mobility in metallic systems3 predicts that the diffusion coefficient for rhenium is less than that experimentally determined for tungsten4 in the temperature region 1500. to 2200°C. At these temperatures the elastic modulus for tungsten5 is only slightly larger than the extrapolated modulus for rhenium.6 Thus, rhenium is a good possibility for a a high-temperature structural material, but few data on the creep of rhenium have been reported. This investigation was undertaken to study the high-tempera-ture deformation behavior of rhenium in detail. EXPERIMENTAL TECHNIQUES The material used in this study was consolidated from high-purity powder. After cold pressing the powder to a plate a in. thick, the billet was sintered in hydrogen at 2250°C for 24 hr. The plate was reduced to 0.100 in. by cold cross rolling with intermediate anneals at 1650°C for 20 min between passes. The plate was further reduced to 0.060 in. by unidirectional cold rolling with similar heat treatments between passes, and then finally stress-relieved in hydrogen at 1650°C for 30 min. Specimens tested at 1900°C and below were pretest-annealed at 1900°C for 2 50 hr. Specimens tested above 1900°C were pretest-annealed at 2400°C for 5 hr. The impurity content in the "as-received" plate was quite low, table I. Essentially no change in impurity levels was detected in specimens after creep testing. All creep tests and annealing treatments were conducted in a vacuum of 10-8 torr in a test furnace heated by a tungsten mesh element. The load was applied to the specimens through a bellows, and stresses were maintained to ±1 pct of the selected value by periodic corrections for changes in specimen cross-sectional area during creep and for changes in the bellows spring force due to load column extension. One-inch-diameter tungsten force rods were used in the hot zone of the furnace. Deformation at temperature was measured by optically tracking gage marks on the specimen. Temperature was measured by a calibrated optical pyrometer and was determined to ±5"C. Grain sizes were determined by the linear intercept method and specimens were examined in the "as-polished" condition, using polarized light. Specimens annealed at 1900°C had a grain size of 52 ± 5µ , and those annealed at 2400°C had a grain size of 148 * 11 µ. Pieces were cut from the gage section of creep-tested specimens and planed to a thickness of about 0.010 in. by spark discharge machining. Thin foils for viewing by transmission electron microscopy were obtained by electropolishing in a solution of 6:3:1 ethyl alcohol, perchloric acid, and butoxy ethanol, respectively, using the window technique. Bath temperature was —4OoC, and the cell potential was 35 v. The foils were examined in Siemens Elmiskop I, operating at 100 kv. RESULTS AND DISCUSSION In order to analyze the results from creep experiments, Eq. [I] is rewritten in the following form: <=Kf(s)ne-/RT [2] where K = constant, ?// = apparent activation energy for creep,

Jan 1, 1970

By D. P. Kedzie, R. A. Dodd

The fatigue strength, fatigue hardening, and effect of fatigue deformation on subsequent age hardening of supersaturated Al(Cu) solid solutions have been determined as functions of alloy composition and temperature. The fatigue strength/tensile strength ratios, determined at 150°, 25°, and -195°C, decreased with increase in alloy content for all temperatures, but the F.S./U.T.S. ratios at -195°C decreased much more rapidly than did the ratios for 150" and 25°C. This suggested that strain aging and/or age hardening occurred during tests at higher temperatures. Additionally, the F.S./U.T.S. ratios at 150°C exceeded those at 25°C for all compositions, indicating greater strengthening during fatigue at 150°C. The effect of fatigue or tensile deformation at 150°, 25°, and -195°C on subsequent age hardening showed that the deformatzon increased the rate of precipitation and indicated that mechanically produced vacancies were probably formed during deformation. Fatigue hardening was studied at 150°, 25°, and -195°C, and the effect of room-temperature rests after 10 and 100 cycles was examined. The results confirmed that strain aging occurred at the higher temperatures . DURING the last 15 years various mechanisms of fatigue crack nucleation and growth based on dislocation and vacancy interactions, operating singly or collectively, have been proposed. The probable consensus of present opinion is that the fatigue process in pure metals essentially involves dislocation interactions, and that vacancies formed by such interactions play a minor or inconsequential role. However, there is some evidence that age-hardened alloys tend to overage during fatigue, probably by local vacancy-enhanced diffusion, and strain aging also might be important in selected cases. Furthermore, it has been established that the behavior of quenched-in vacancies in Al(Cu) and other solid solutions is composition-sensitive. Therefore, it seemed worthwhile to investigate various aspects of the fatigue behavior of supersaturated Al(Cu) alloys and to examine the results in terms of vacancy-enhanced effects. EXPERIMENTAL The alloys used in this investigation were prepared from 99.994 wt pet A1 and OFHC copper, the latter containing 0.04 pet 0 as the principal impurity. Six alloys were made, containing, by actual analysis, 0.58, 0.96, 1.96, 2.85, 4.45, and 5.51 wt pet Cu. They were induction-melted in air in graphite crucibles, cast as 7-in. by 7/8-in.-diam rods in graphite molds, and hot-rolled to 5/8 in. diam. The experimental work was a three-part program involving the determination of a) 10&apos; cycle fatigue stresses as a function of alloy composition and temperature; b) the effect of fatigue deformation on subsequent aging of the supersaturated alloys; and c) fatigue hardening as a function of alloy composition and temperature. For determining the 105 cycle fatigue stresses, a portion of the 5/8-in. stock was machined into Krouse rotating cantilever beam fatigue specimens, 2 in. in length by 1/4 in. minimum diameter. These were tested at +150°, 25°, and -195°C (liquid nitrogen) on a Krouse high-speed machine, with special weights to provide lower -than-normal loading ranges, this being necessitated by the small load requirements of those alloys of lower copper content. For the high-temperature tests a small resistance heater was designed to clear the collets and fit in between the chucks, while for the low-temperature tests a hollow nylon cylinder was used, having closed ends drilled to pass a fatigue specimen, and positioned similarly to the heater. A plexiglass container completely enclosed the fatigue machine; rubber gloves fixed to ports in the walls enabled the machine to be operated from outside the box. A tray of magnesium perchlorate dried the air in the container and prevented both atmospheric corrosion fatigue at room and elevated temperatures and troublesome ice build-up at low temperatures. A total of ten to fifteen specimens was used for each combination of alloy composition and temperature. The result of each test was plotted on a standard S-N diagram, and the next stress was selected on the basis of the trends indicated by previous specimens. In this manner a small portion of the S-N diagram was constructed, and the 105 cycle fatigue stress obtained. Small Krouse fatigue specimens were also used to study the effect of cyclic prestrain on subsequent

Jan 1, 1964

By T. P. Chen, F. W. Bowdish

Studies made with a captive bubble apparatus on the sulfidization and collection by amyl xanthate of true chrysocolla specimens have defined the ranges of pH value and sulfide concentration which permit contact between the bubble and the mineral surface. Titanium compounds were the most effective of the materials found to activate the sulfidization of chrysocolla. With titanium activation, the contact angles and the ranges of pH value and sulfide wncentration giving bubble contact were all increased. Chrysocolla ores were concentrated by flotation. Chrysocolla ores occur at many localities in grade and quantity sufficient to make mining and millin feasible, but no satisfactory method of concentratio has been found. Although chrysocolla may be leached with acid, only those ores without acid-consuming gangue may be leached economically. Because of its potential importance, a study of the conditions nece sary for flotation of chrysocolla has been carried ou The literature contains a few references to flotation of chrysocolla. Two methods were developed by the U. S. Bureau of Mines.1,2 The first consisted of a fatty acid soap and a high xanthate as collectors of chrysocolla from a synthetic ore, while the second involved the use of hydrogen sulfide and xanthate. Ludt and DeWitt3 demonstrated the difference in adsorptive powers of chrysocolla and quartz for bas triphenyl methane dyes and suggested the use of butyl, hexyl or octyl-substituted malachite green as collector. Jackel4 emphasized the effects of combin tions of reagents such as Aerofloat 31, pine oil, and Reagents 404 and 425 with sodium sulfide and zinc hydrosulfite as conditioning agents. Although he reported recoveries of 89% from a synthetic ore and 98% from a natural ore containing azurite, malachite, chalcopyrite and chrysocolla, careful application of Jackel&apos;s method to chrysocolla from Tyrone, N.M., failed to give a high recovery. MATERIALS AND TECHNIQUE Samples from Inspiration, Ariz., and Tyrone and Magdalena, N. M., were used for experimentation and verified as true chrysocolla by leaching tests, specific gravity tests and X-ray diffraction. Chrysocolla does not dissolve at pH 4, although malachite and azurite do. Chrysocolla is about half as dense as the copper carbonates. X-ray diffraction analyses by the powder camera method confirmed the samples as true chrysocolla. A captive bubble apparatus, which cast an enlarged image of the air bubble and the mineral surface upon a screen, was used to check on the character of the surfaces. The specimens were prepared by grinding a flat surface on a glass plate using fine abrasive; then they were washed and kept in distilled water until they were to be treated with reagents. Before each reagent treatment, the specimen was carefully checked for cleanliness in the captive bubble apparatus. It was assumed that the surface was clean if, after fine grinding and washing of the specimen, the bubble would not stick. Specimens were handled with glass forceps, and precautions were taken to avoid contamination of the mineral surfaces. Contact angle measurements were carefully made several times on each treated specimen to obtain reliable average values. EFFECT OF pH VALUE AND SODIUM SULFIDE CONCENTRATION In each experiment, a specimen with a freshly ground surface was immersed for 10 min in a solution of sodium sulfide, washed and immersed for 15 min in a solution containing 30 mg per 1 of potassium amyl xanthate. The specimen was then washed again in distilled water and tested for contact angle in the captive bubble apparatus while submerged in distilled water. In this series of experiments, the pH of the sulfidizing solution was varied from 3 to 7, and the concentration of sodium sulfide, containing 60% Na2S, was varied from 50 to 650 mg per 1. Many combinations of pH value and sulfide concentration resulted in no contact between the bubble and the surface, but over a limited range of conditions, contact angles varying from 24ºto 52ºwere obtained. The data in Fig. 1 show sulfidization conditions that lead to bubble contact and those that do not. The region of contact is surprisingly small, which may indicate why flotation of chrysocolla involving sulfidization has proven so difficult in practice. Several features of the system are illustrated in Fig. 1. In the region between pH values of 4 and 6 with sodium sulfide concentrations below about 350

Jan 1, 1963

By L. O. Bacon

IN the spring of 1952 Calumet and Hecla Inc. began a geophysical program near Shullsburg, Wis., in the Wisconsin-Illinois lead-zinc district, to assist the geological and drilling exploration programs. Sphalerite, the ore mineral in this area, occurs with a considerable amount of marcasite. In general the higher the percentage of sphalerite in the ore, the higher the percentage of marcasite; however, there may be mineralized zones high in marcasite but low in sphalerite. Orebodies in general are relatively narrow and elongated. Reconnaissance exploration of virgin areas consisted of drilling along lines at 500 to 1000-ft intervals. Whenever a mineralized zone was intersected additional drilling was done to determine whether or not the zone carried zinc percentages of ore grade and, if so, to delineate the body. Calumet and Hecla Inc. was interested particularly in a method that would show the direction and position in which to drill from the original discovery hole. This suggested a method of contacting the orebody, which occurs at depths ranging from 100 to 200 ft, with one electrode. After a number of procedures had been considered it was decided to use equipotential line methods. Instrumentation and Field Procedure: The power source used was a 400-cycle Signal Corps motor-generator having a rated output of 1200 w at 115 v. The detection unit consisted of test probes, a two-stage amplifier, and &apos;head phones for determining the equipotential line by audio null. Field procedure consisted of contacting the sulfide body in the hole by a specially built spring-loaded expanding electrode which would be lowered into the hole, in the closed. position, until it reached the mineralized zone. At that point the mechanism was released so that the arms would make contact with the walls of the hole in the same manner that a well-bore caliper does. This electrode was then connected to the generator, the other terminal of which was connected to the surface electrode. The surface electrode was either a point, a straight line, or a circular line electrode. The point surface electrode was placed at a considerable distance from the hole, that is, 2500 to 5000 ft, depending somewhat upon the depth to the sulfide zone and the distance from the hole containing the subsurface electrode to which exploration was considered. A higher voltage output from the power source would have been desirable, although no difficulty was encountered in determining null points to a distance of 500 ft. Straight line electrodes used were approximately 1000 ft in length at a distance of approximately 1000 ft from the hole containing the subsurface electrode. The circular line electrode used consisted of 4400 ft of bare No. 10 copper wire, which provided a circle of 700-ft radius. All line electrodes were fastened to the ground at 20-ft intervals with copper staples 4 in. long. Equipotential points were determined at 25 to 100-ft intervals. Location of the points was made by plane table and stadia. In open country with a three-man crew, the points were plotted as they were determined. With a two-man crew, pegs were placed at equal potential points and surveyed in after several equipotential lines were determined. Although interpretation of results given in this paper is qualitative, the paper as a whole would not be complete without a discussion of the theoretical distribution of potential due to a circular line electrode. The theoretical distribution would be required if a quantitative interpretation of the measured potential distribution were to be made. The theoretical potential distribution due to a circular line electrode can be obtained by means of Legendre polynomials. Using the method as developed by Weber,&apos; the potential for a circular line electrode in a semi-infinite, homogeneous, isotropic medium can be expressed, using the spherical coordinate system, as: V(r,n) = pi/2pR[S(r/R)nPn(cos?)Pn(cosa)]r<R [1] er V(r,a) =pI/2pr[S(r/R)Pn(cos?) Pn(cosa)]r>R [2] where: 0 is the angle at the origin, taken on the axis of the circular electrode between the axis and the line drawn to the circumference of the circular electrode. a is the angle between the axis and the radius, r.

Jan 1, 1957

By Joseph C. Mead, Alan Stanley

The MacIntyre Development of the National Lead Co. is located at Tahawus, N. Y. The operations involve the mining and concentrating of a titaniferous iron ore to produce an ilmenite concentrate and a magnetite concentrate. Construction of the MacIntyre plant was commenced during the summer of 1941,when world conditions threatened to cut off the supply of Indian ilmenite. An open pit mining operation was developed and the crushing and milling equipment put in operation in July 1942. A general description of the operation was given in the Adirondack Issue of Mining and Metallurgy for November 1943. The metallurgy of the mill operation was described by Mr. Frank R. Milliken,* Plant Manager, National Lead Company, MacIntyre Development, and presented at the AIME New York Meeting, February 1948. The magnetite concentrate produced in the milling operation was too fine (minus 20 mesh) to be used directly in iron blast furnace operation, and most of the magnetite had to be stockpiled in 1942 and 1943. In 1943, the Defense Plant Corp. built a Greenawalt sintering plant at Tahawus, N. Y., to put the magnetite concentrate in a more suitable form for use in the iron blast furnace. The Greenawalt sintering plant consists of three 10 by 25 ft sintering pans designed to produce 1800 gross tons of sinter per 24 hr. The vacuum to each pan is produced by two Greenawalt fans in series, pulling approximately 30,000 cu ft of air per minute at 50 in. water gauge vacuum. The plant started operation in August 1944. The present plant production averages 25 tons per operating pan hour (approximately 224 lb per operating hour per square foot of grate area) of plus 1 in. sinter. Raw feed to the plant consists of 61 pct magnetite, 4 pct anthracite coal culm, and 35 pct minus 1 in. return fines which are conveyed to a pug mill where the materials are mixed thoroughly and water added to give the mixture 5.5 to 6 pct moisture. The mixed prepared feed is conveyed to two 4 by 10 ft vibrating screens where the minus 1 in. plus 5/8 in. return fines are screened out and discharged into a surge bin for use as a hearth layer. The minus 5/8 in. prepared feed is discharged into another surge bin for use as prepared feed. A charge car, electrically operated, having a capacity of one charge of prepared feed and several charges of hearth layer, lays a thin layer of plus 5/8 in. return fines and 9½ in. depth of prepared feed into the pans. A fluffing roll and a vibrator on the car fluffs and spreads the prepared feed into the pans. An ignition car, electrically operated, ignites the top of the bed with a 30 sec flash burn. The 9½ in. bed sin-ters in approximately 13 min. Dumping the pan, and recharging and igniting the bed requires 2 min. To improve the quality of the ilmenite concentrate produced in the mill and to reduce the amount of titanium dioxide lost in the mill tailings and in the magnetite product, extensive research work and pilot plant operations have been done on grinding the crude ore to minus 65 mesh size (rather than to minus 20 mesh) and concentrating it by a combination of magnetic separation (for magnetite recovery) and flotation (for ilmenite re-covery). These tests have proved successful in increasing ilmenite re-covery and grade. With the development of the ilmenite flotation process to a stage where a full scale flotation plant was in the design stage, the problem arose of handling the 65 mesh magnetite concentrate that would be produced. In order to study and solve the problems of handling and sintering the 65 mesh magnetite in the sinter plant, a pilot sinter plant was secured from John E. Greenawalt. The effect of using 65 mesh magnetite in the sintering operations was then studied on the 2.4 sq ft test pan, operating under conditions as similar to the large plant as could be set up in the laboratory. A series of tests were run in the test pan on present sinter plant feed that had been mixed in the plant pug mill. An average production and an average quality of sinter produced in this series

Jan 1, 1950

Abdul-Ahad. A., Student, Montana School of Mines, Residence Hall Butte, Mont. &apos;39 Abramovits, Charles, Student, Case School of Applied Science Cleveland, Ohio. &apos;37 Abreu, Ovidio M., Student, Univ. of Nevada Reno, Nev. &apos;38 Acker, Voscoe, Student, Agricultural & Mech. College of Texas College Station, Tex. &apos;39 Adams, Albert, Student, New Mexico School of Mines Socorro. N. M. &apos;38 Adams, Charles W., Student, Michigan College of Min. & Tech Houghton, Mich. &apos;39 Adams, Hugh T., Jr., Student, Univ, of Oklahoma Norman, Okla. &apos;39 Adams, Jack L., Student, Univ. of Oklahoma Norman, Okla. &apos;39 Adams, Jack M., Student, Univ of Alaska College, Alaska. &apos;39 Adams, Lewis J., Student, Agricultural & Mech. College of Texas, Box 2514, College Station, Tex. &apos;39 Adams, Robert E., Research Engr., Battelle Memorial Inst Columbus, Ohio. &apos;38 Adamson, George M., Jr.. Student, Univ. of Utah Salt Lake City, Utah. &apos;39 Adkisson, J. F., Jr., Student, Agricultural & Mech. College of Texas, Box 1003, College Station. Tex. &apos;38

Jan 1, 1939

By Mark J. Klein, A. H. Clauer

The Snoek peak induced by solute nitrogen in chromium was studied. A rapid quenching rate is required to maintain nitvogen in solution in sufficient concentrations to be detectable by internal-friction techniques. An expression for the tertninal solubility, c, of nitrogen in weight pevcent is log,,c = -4130/T + 1.05. The diffusion of nitrogen in zhromium determined by internal friction is SNOEK&apos;S theory1 of the stress-induced ordering of interstitial solute elements in the bcc lattice has been used to deduce information on the behavior of interstitials in a number of bcc metals. Under the proper conditions, internal-friction studies of "Snoek peaks" permit a determination of diffu-sivities, solubilities, and precipitation kinetics of interstitial elements. Internal-friction studies of this type have been reviewed by Nowick,&apos; Wert,= Powers and Doyle,4 and others. The behavior of interstitial atoms in Group V-A metals and iron has been rather extensively studied in this way, and results are reasonably self-consistent. However, the study of interstitial elements using internal friction in the Group VI-A metals—tungsten, molybdenum, and chromium—is much less clear. Thus far, internal-friction studies have revealed a peak in tungsten tentatively attributed to carbon5 and a peak in chromium associated with nitrogen. In chromium, Bungardt and Preisendanz6 observed a peak at 180°C for a frequency of -1 cps which they associated with nitrogen. More recently, de Morton7 determined the diffusivity of nitrogen in chromium from studies of a nitrogen peak at 160°c for a frequency of -1 cps and from elastic aftereffect measurements. The objective of this investigation was to study the nitrogen peak in greater detail, to obtain information on the behavior of nitrogen in chromium. This information is of interest because nitrogen is known to have an embrittling effect on chromium. However, efforts to deduce the role played by nitrogen in influencing the mechanical behavior of chromium are handicapped by lack of information on its behavior and distribution in chromium. EXPERIMENTAL PROCEDURES The chromium wires used in these studies were drawn from arc-melted iodide-chromium stock that had been extruded, swaged, and centerless-ground to 0.25 in.-diameter rods. Internal-friction measurements were made in an evacuated torsional pendulum similar to the one described by Kê,8 utilizing wires 0.048 to 0.030 in. in diameter. A series of analyses of the fabricated wires showed that the major impurities were approximately 100 ppm Fe and a combined interstitial content of 50 to 100 ppm C, O, N, and H. A typical interstitial analysis of the wires after processing is 15 ppm C, 2 ppm H, 50 ppm O, and < 5 ppm N. Interstitial concentrations were determined by vacuum-fusion, combustion-conductimetric, and micro-Kjeldahl analyses. In general, vacuum-fusion analysis yielded a lower nitrogen concentration than did micro-Kjeldahl analysis. For consistency, the nitrogen concentrations reported in this investigation were determined by the former method. Heat treatments were carried out by encapsulating the specimens in quartz tubes containing argon. The fabricated wires were annealed at 1150°C for 1 hr to produce uniform recrystallized grain size of about 0.015 mm. Nitrogen and carbon were added to the fabricated wires by encapsulating them in a quartz tube containing ammonia or methane, and annealing them at 1150°C for 48 hr. In some instances, carbon was also introduced by coating the wires with carbon black prior to annealing.

Jan 1, 1965