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By AIME AIME

The following persons have been proposed for election as members or associates of the Institute during March and April, 1908. Their names are published for the information of members and associates, from whom the Committee on Membership earnestly invites confidential communications, favorable or unfavorable, concerning these candidates. A sufficient period (varying in the discretion of the Committee, according to the residence of the candidate) will be allowed for the reception of such communications, before any action upon these names by the Committee. After the lapse of this period, the Committee will recommend action by the Council, which has the power of final election.

Jan 5, 1908

By Charles E. Mauk, H. William Prengle, Robert W. Legan

A process breakthrough was needed for the complete destruction of total cyanide influent as high as 100,000 mg per 1, or below 1 mg per 1, to produce an influent with total cyanide below the limit of detection. The process uses ozone for the total destruction of cyanide and metal cyanide complexes. It was found that while ozone alone reacted with the iron cyanide complexes too slowly for practical application, ozone at slightly elevated temperature became more effective, and ozone with ultraviolet light became effective enough to permit the design of a successful system.

Jan 1, 1977

By J. French Robinson

A review of production in the Eastern District for 1930 is necessarily brief. Drilling operations were curtailed, due to economic conditions, which in turn reduced production. However, in spite of these conditions, there have been a few outstanding developments which surpass any of recent years. The development of a field in Chautauqua and Cattaraugus counties, New York, has been rapid and probably reached its peak of production in 1930. The gas in this field comes from the White Medina Sand (Silurian), at an average depth of 2600 ft. Some of the wells had an open flow of 20,000,000 cu. ft. of gas per day,' with an original rock pressure of 965 pounds2 per square inch. Another area developed during 1930 was the Tyrone field, in Tyrone Township, Schuyler County, New York. This field was discovered 2nd is practically controlled by the Belmont Quadrangle Drilling Corpn. of New York. The production is from the Oriskany Sand (Devonian), which is found at an average depth of 2100 ft. The field covers approximately 2000 acres, and to date has 14 producing gas wells. The largest well had an open flow of 15,000,000 cu. ft. and an original rock pressure of 740 Ib. The gas from this field is impregnated with sulfur, and requires washing before it is marketed. Because little is known of the Oriskany Sand, a brief description may be of interest. This sand outcrops at Oriskany Falls, New York, and has a thickness of 10 to 12 ft. Its texture is coarse grained, it is composed mostly of quartz and is a regularly bedded sandstone. At Yauger's Wood, in Cayuga County, New York, it is exposed and shows a thickness of 26 feet. The discovery of the Tyrone field led to much prospecting in the New York and the northern part of Pennsylvania, and as a result of this search, the Allegany Gas Co. struck a large gas well in Farmington Township, Tioga County, Pennsylvania, which created considerable excitement through the Eastern District. The gas was encountered at a depth of 4010 ft., and tested 20,000,000 cu. ft. open flow, with a shut-in pressure

Jan 1, 1931

By W. S. Ayres

The construction of a new breaker at the Cranberry Colliery, Hazleton, Pa., was forced upon the operators, A. Pnrdee & Co., by a fire which destroyed the entire plant early in January, 1896. The loss included, in addition to the breaker, three boilerhouses and three engine-houses. The boilers were not injured, but the steam-pipes and connections were all broken and warped by the fire. The boilers were probably saved from injury by the presence of mind of the fireman., who started all his feed-pumps and filled the boilers with water. The hoisting-engines were more or less warped and cracked, but by patching and replacing the injured and broken parts, they were made to do satisfactory service in the new plant. It may be worthy of mention that the wrought-iron shaft of one of the hoisting-drums, 12 inches in diameter by 17 feet long, was so heated in the fire that the weight of the drum caused it

Jan 1, 1899

By Peretti, E. A.

Since its development about forty years ago by J. V. N. Dorr (Cyanidation and Concentration of Gold and Silver Ores, McGraw Hill Book Co., 1936, 1-5), and others, continuous countercurrent decantation has not only become one of the standard methods for extracting gold and silver from their ores, but has also found wide application in other metallurgical and chemical industries. In 1917 L. B. Eames published an excellent paper (Countercurrent Decantation, Trans AIME, 1917, 57, 143- 158), in which he determined the effects of grade of ore, ratio of solution precipitated to ore treated, variations in the density of the thickener spigot discharge and variations in the value of the barren solution upon the gold assay of the solutions discharged from the thickeners in the system. Eames showed that, other things being equal, the dissolved gold lost in the tailing varies directly as the value of the ore and as the value of the barren solution. The tailing loss de- creases rapidly as the ratio of solution precipitated to ore treated is increased to about three or four to one. Beyond this point the improvement is negligible.

Jan 1, 1949

By Richmond Bennett

Airborne geochemistry became a reality with the advent of a high-sensitivity air¬borne gamma ray spectrometer with large volume NAI(Tl) crystal detectors. The high-sensitivity spectrometer measures small variations in the concentration of potassium (as Ks°), thorium (as Tl308) and uranium (as Bi.214) along the flight lines in the area surveyed. Hydrothermal dispersion patterns are indicated by anomalous measured values of the concentrations of potassium, thorium, uranium, or their ratios. In two recent Australian survey areas, copper mineralization was located along favorable structures within hydrothermal dispersion patterns delineated by airborne geochemical surveys. In metamorphic terrane where there had been po¬tassium metasomatism, the hydrothermal dispersion patterns were indicated by high potassium/uranium ratios (K40/Bi). In a sedimentary environment that had been intruded by a stock, the path of hydrothermal fluids was indicated by uranium (Bi214), thorium (TV'), and uranium/ thorium (Bi214/Tl208) ratios.

Jan 1, 1972

By Arthur F. Taggart

A general awakening of interest among mill men concerning the mechanical efficiencies of their crushing machines is evident from a perusal of the recent files of mining publications. Considering the large part of the power bill which must be debited to the crushing department, such interest is natural. When, however, the articles on the subject are read, the only statement upon which the writers agree is that fine grinding consumes a large amount of power, and that the machine which, from a concentration standpoint, offends as a slime producer is, for that reason, a serious offender in wasting power. When the mill man attempts to find a method for measuring the power wasted, or to compare the efficiency of one machine with that of another for the same work, he is confronted with a choice of methods which lead to conflicting results. There are two reasons why the work of crushing is not more generally understood. In the first place, experimental data are difficult to obtain; and in the second place, before these data can be put in general form certain assumptions must be made. A difference in these assumptions by different investigators has led to conflicting conclusions. This conflict has resulted in the proposal of two laws. The first of these is the so-called Rittinger's law, which is variously stated as follows: "The work of crushing is proportional to the reduction in diameter."—R. H. Richards: Ore Dressing, p. 304 (1903). "The work required to crush rock is very nearly proportional to the reciprocals of the diameters crushed to."—A. Del Mar: Engineering and Mining Journal, vol. xciv, No. 24, p. 1129 (Dec. 14, 1912). "The work done in crushing is proportional to the surface exposed by the operation, or better expressed for this purpose, the work done on a given mass of rock is proportional to the reciprocal of the diameter of the final product, assuming that all the mass has been reduced to one exact size, which is only theoretically possible."— A. 0. Gates: Engineering and Mining Journal, vol. xcv, No. 21, p. 1039 (May 24, 1913). ' ' " Of this law as variously stated above H. Stadler says (Grading Analyses and Their Application, Author's Reply to Discussion, Transactions of the Institution of Mining and Metallurgy, vol. xx, p. 426 [1910-111):

Jan 1, 1915

By Edward Wichers

THE purpose of this paper is to set forth the matters of principal interest in connection with work done in the past few years on the purification of the metals of the platinum group, including the study and modification of methods already in the literature and the development of new procedures. For the most part, the results will be given in summary form, reserving the publication of detailed data and directions for a forthcoming paper to be issued by the Bureau of Standards. In recent years increasing interest has been shown in the preparation of the pure platinum metals, both by those concerned with the manufacture of the metals and their alloys for scientific and industrial purposes and those who are engaged in the study of the chemical or physical properties of the elements. The purification of the metals usually has been regarded as a matter so involved and difficult as to require the attention of specialists. It is hoped that this paper will show that any of the metals can be prepared in any desired degree of purity by relatively simple straightforward chemical methods. For the most part, it is thought that the methods given are suitable for small-scale refineries as well as for the laboratory; also, that they will bring the time required for the purification of any of the metals within reasonable limits. The new procedure suggested for purifying platinum should prove to be much shorter than any methods described in the literature.

Jan 1, 1928

By Edward Wichers

THE purpose of this paper is to set forth the matters of principal interest in connection with work done in the past few years on the purification of the metals of the platinum group, including the study and modification of methods already in the literature and the development of new procedures. For the most part, the results will be given in summary form, reserving the publication of detailed data and directions for a forthcoming paper to be issued by the Bureau of Standards. In recent years increasing interest has been shown in the preparation of the pure platinum metals, both by those concerned with the manufacture of the metals and their alloys for scientific and industrial purposes and those who are engaged in the study of the chemical or physical properties of the elements. The purification of the metals usually has been regarded as a matter so involved and difficult as to require the attention of specialists. It is hoped that this paper will show that any of the metals can be prepared in any desired degree of purity by relatively simple straightforward chemical methods. For the most part, it is thought that the methods given are suitable for small-scale refineries as well as for the laboratory; also, that they will bring the time required for the purification of any of the metals within reasonable limits. The new procedure suggested for purifying platinum should prove to be much shorter than any methods described in the literature.

Jan 1, 1928

By R. W. Smith, M. E. Brookes

The temperature at which th: quenched 0' (ordered bcc) phase transfo.rms to the ( (complex hexagonal) phase on heating has been examined for certain Ag-Zn and Ag-Au-Zn alloys using an electrical resistivity method. The transition temperature decreases by approxinzately 7°C as the zinc content is reduced by 1 at. pct. The critical temperature, Tc, for long-range order has also been measured for a number of Ag-Au-Zn alloys. Extrapolation to zero gold content suggests that Tc decreases by approximately 5°C per 1 at. pct reduction in zinc content. The 0 phase of the Ag-Zn system exists over a narrow range near the composition Ag zn,' Fig. 1, and has a bcc structure which is disordered above 272°C. Slow cooling to temperatures below the range 274"/258"C allows the complex hexagonal phase, r° to form.2 This is the stable structure at room temperature.3 Upon quenching 0 -phase alloys from high temperatures, it is found that the 0 — (' transformation is suppressed; but ordering takes place (i.e., 0 -0'). This ordered structure can also be obtained by the room-temperature aging of cold-worked (0.4 Deformation of the 0' phase gives rise to a fur- ther hexagonal phase ( (of nearly ideal axial ratio) which reverts to b' within a few hours.= In view of this, it has been suggested that the equilibrium struc-

Jan 1, 1969

By N. Jaffee, J. E. Dorn

An activation energy of 27,400 5 1000 cal per mole was obtained for the creep of poly crystaLline aluminum over the temperature range of 273° to 350°K, at strains varying from 0.003 to 0.230. Stresses varied fronz 2250 to 6000 psi, strain rates from 0.1145 x 10-5 to 29.5 x 10~s min.-1. A strain temperature-compensated time correlatzon was oblained indicating that the structure was depedent solely upon the strain at a given stress; X-ray diffraction analyses and tensile tests on precrept specimens verified this. PREVIOUS investigations1 have revealed that the apparent activation energies for creep of high-purity polycrystalline aluminum are insensitive to the applied stress, strain, and strain rate. On the other hand, the apparent activation energy is dependent on the temperature1,2 as shown by the data reproduced in Fig. 1. Each plateau of this curve is associated with a unique rate-controlling dislocation mechanism for thermally activated creep. It is now very well-established that over the high-temperature range, where the activation energy is about 35,500 cal per mole, the creep rate is controlled by the dislocation climb mechanism. 3 Over the intermediate range of temperatures, from about 260° to 370°K, another unique activation energy, namely 28,000 cal per mole, is obtained. Current evidence strongly supports the contention that cross slip is the rate controlling mechanism for creep in this case: 1) Crystal recovery can occur by a number of mechanisms prominent among which are climb and cross slip. Astrom,4 using the Borelius micro-calorimeter, reported rapid crystal recovery of cold-worked polycrystalline A1 at 340° to 370°K giving an activation energy of 28,000 cal per mole and additional recovery at 455° to 478°K giving an activation energy of 3 6,000 cal per mole. Whereas the latter recovery process was clearly associated with the dislocation climb mechanism, the former, 28,000 cal per mole process could have arisen as a result of the cross-slip mechanism. 2) Single crystals of high-purity A1 favorably oriented for octahedral glide exhibit an activation energy for creep of about 3400 cal per mole over the range from 0° to 400°K and that of about 28,O:O cal per mole over the range from 600° to 775°K . Whereas the lower activation energy process is accompanied by the development of sharp slip-band traces, the 28,000 cal per mole process was uniquely characterized by extensive cross slip. 3) Theoretical calculations by Seeger and schoeck6 suggest an apparent activation energy for cross slip in A1 of about 24,000 cal per mole and another theoretical estimate by Friedel 7 gives the observed 28,000 cal per mole as the theoretical activation energy. It is therefore consistent with this evidence to, at least tentatively, ascribe the 28,000 cal per mole creep process in A1 to the operation of cross slip as the rate controlling mechanism. Although creep has been rather well-explored in the dislocation climb range, very little, excepting perhaps the activation energy, is known about creep in the cross slip range. This investigation was undertaken, therefore, to reconfirm the activation energy for creep in polycrystalline A1 in the intermediate temperature range and to study the strain-time relationship for creep at a constant stress in the cross slip region. EXPERIMENTAL PROCEDURE AND TECHNIQUE The three types of high-purity A1 alloy specimens described in Table I were used in this investigation. Specimens were milled from 0.100 in. thick cold-rolled sheets with their tensile axes in the rolling direction following which they were given a recrys-tallization and grain growth heat treatment at temperatures well above those which were subsequently employed in the creep tests.

Jan 1, 1962

By C. Pin, J. Bruce Wagner

In order to demonstrate the role of defect chemistry in the solid state to a process-metallurgy reaction, laboratory experiments were carried aut to remove copper from liquid lead using lead sulfide which had been doped to provide definite concentrations of cation vacancies. The removal of copper decreases in the order: bismuth- or antimony-doped PbS, undoped PbS or tin-doped PbS, and silver-doped PbS. The data are explained using the simple mass -action law and in terms of the exceedingly rapid interstitial diffusion of coppw in PbS to vacant cation sites. Results are in agree-ment with thermodynamic predictions and certain industrial practices that copper may be removed from lead below the limit of its coexistence with pure Cu,S and pure PbS. The role of defects in solids has been exploited in semiconductors and many device applications, in explaining tarnish formation, dissolution rates, and mechanical properties. The application of these principles to many process-metallurgical problems has not received as much attention. It was the purpose of this study to illustrate the role of defect structures of solids in a process-metallurgical application. When lead is refined, the ore, galena (PbS), is reduced by a series of operations to liquid lead (lead bullion) containing impurities such as copper, bismuth, antimony, arsenic, and silver depending on the original composition, the fluxes added, and the particular type of operation, see Fig. 1. In order to produce a pure lead, a series of refining operations are carried out. A typical lead-bullion analysis before drossing is shown in Table I. Copper is removed first as its presence increases the zinc consumption during the desilverizing process. For preliminary copper removal the lead bullion is brought to a temperature of 440°C in a kettle of 60 metric tons capacity. Some tar (or sawdust or resins) is usually added and the kettle is cooled slowly to 400°C while the liquid is stirred. A solid phase, called a dross, floats on top of the liquid and the particles of the solid phase adhere to the tar. This "hot dross" is collected. It contains mostly lead and copper which are partly oxidized and/or sulfurized if the lead bullion contains some sulfur.*

Jan 1, 1963

By H. Scott

Since Bohler discovered, in 1903, on cooling certain alloy steels, the phenomenon of a new and lower temperature transformation than the usual Ar 3-2-1 obtained by increasing the maximum temperature to which the material was heated, much has been published1 connecting this phenomenon with a large number of dissimilar steels of high alloy content. From the fact that the transformation divides itself, taking place at two widely separated temperatures, it has been called a "split transformation." The significant facts established by recent investigators2 are: that when the transformation occurs at the higher temperature Ar1, troostite or a decomposition product is formed, and that when the transformation occurs at the lower temperature Ar", the resulting structure is martensite. The terminology Ar' and Ar" adopted here is that of Portevin. Previous Investigations Reviewing the work on this subject published in a recent issue of Revue de Metallurgie and referring in particular to his statement that martensite is a solution of carbide in alpha iron, Le Chatelier says :4 "How then can a theory already 20 years old demand new investigations? The reason for it is that we have not succeeded in proving directly the real presence of the transformation of iron during the very short duration of the quenching. The fall of temperature takes place at the rate of several hundred degrees per second and the observation of

Jan 1, 1920

By R. M. Hudson

The removal of nitrogen from a nitrogenized low-carbon sheet steel that contained 0.011 wt pct N was determined during heat treatment in Hz-N, mixtures. TIze process followed a first-order rate law; that is, plots of the logarithm of nitrogen content in steel were linear with the time of treatment at a given temperature. The rate of removal increased with an increase in temperature from 900" to 1300°F. By 1400°F the rate in dry hydrogen had decreased to a value intermediate between the rates at 1200" and at 1300°F; in wet (2.47 vol pct water vapor) hydrogen the rate at 1400°F was less than the rate at 1300°F and nearly the same as the rate at 1200OF. The rate at a given temperature increased as the 3/2 power of hydrogen concentration in the atmosphere. While wet atmosplzeres were generally more effective than the corresponding dry atmosplzeres, the effect of water vapor was much less pronounced than the influence of hydrogen content. NITROGEN is the principal agent in the strain aging of ferrite, the effect of carbon being secondary.' To eliminate the return of the yield point after straining and aging, it is claimed2 that the amount of nitrogen in solution in steel must be reduced to 0.0002 wt pct. Strong nitride-forming elements (titanium, vanadium, zirconium, and aluminum) can act to eliminate strain aging by combining with nitrogen. It is extremely difficult to decrease the nitrogen content in commercial steels to the low level required by conventional coil annealing because of the poor contact between the strip surface and the reactive atmosphere. However, a variety of gas-metal reactions can be effected by use of the open-coil annealing method,3 in which the metal surface is fully exposed to the atmosphere. With this possibility in mind, the Applied Research Laboratory has studied the influence of time, temperature, and atmosphere composition on the removal of nitrogen from low-carbon sheet steel. MATERIALS AND EXPERIMENTAL WORK Samples from a commercial nitrogenized low-carbon steel (0.010 in. thick) in the cold-reduced condition were used. The chemical composition of this steel is given in Table I. The gas mixtures used are listed in Table 11. The moisture content in the "wet" annealing atmospheres was controlled at a +70°F dew point (2.47 vol pct water vapor) by passing the gas mixture through a glass tube packed with a solid mixture of 10 pct anhydrous oxalic acid and 90 pct oxalic acid dihydrate held at 127°F; this technique has been described previously.4 For "dry" atmospheres, the gas mixtures were passed through a cold trap immersed in liquid nitrogen. A hinged-top Hevi-Duty electric furnace was used with a Vycor-glass furnace tube. When the furnace was at the desired temperature, the gas mixture was passed through the furnace at a flow rate between 1.1 and 1.2 cfh; coupons (size 3 by 3/4 in.) of the steel were pulled into the center of the Vycor-glass

Jan 1, 1964

By Ken Sublette

The mining industry has been a leader in the application of ultrasonic level monitoring systems, utilizing the "sonar-in-air" concept for the accurate inventorying of material not only as an end within itself, but going on to activate alarms, turn off feeders, operate tripper systems, and totalize the inventory in numerous bins as well as other more sophisticated applications. The virtues of ultrasonic level monitoring are no doubt appreciated by most users. However, to be of maximum service to the expanding mining industry, the manufacturer must be fair in pointing out ultrasonic's limitations as well as its virtues. The limitations can be surmounted with new technology and through a proper understanding of the principles of operation and application.

Jan 6, 1974

By H. R. Hanley

ONE of the most important contributions to the art of electrolytic zinc production-has been the aluminum cathode. This has been used in all major production: since its commercial development in 1916. The literature is replete with important contributions, some of which may have been replaced by better ones, but thus far there appears no other metal to take the place of aluminum as cathode material. Credit for this innovation goes to Sherard Cowper Coles, of England. When experi-menting on the extraction of-zinc from Broken Hill ore at Hayle, Cornwall, in 1893, he introduced the aluminum cathode, and in 1895 obtained British Patent-No. 20073. The reason for this dominant position of aluminum as cathode mate-rial in zinc sulphate electrolytes is its unique surface, to which electro-deposited metals usually do not tightly adhere. The metal must be of high purity for best results. It is possible to develop a starting-sheet method by which thin electro-deposited sheets of cathode zinc are made and stripped from a smooth aluminum plate. Such thin sheets of cathode zinc may be used as arc tine copper sheets in standard electrolytic copper-refinery practice. However, complications arise because of extreme warping of the zinc starting sheet after a .few hours of deposition, and thus special arrangements must be made to compensate for this abnormality.

Jan 1, 1938

President Howe : It is not so clear to me that the facts which Dr. Waldo brings forward really argue that the nature of the combination between copper and aluminum differs from that of the combination between copper and zinc or copper and tin. As regards electric conductivity, I suppose that the fact, which he thinks points to a special intimate kind of union between aluminum and copper, is that the line in his Fig. 1 is neither straight nor uniformly curved, but that its curvature varies rapidly, not to say abruptly. But we find just such variation in like curves for the copper-zinc and copper-tin alloys. Thus, a slight addition of zinc or tin to copper causes a change in color wholly out of proportion to the quantity added; and, as we add zinc or tin to copper, the tenacity rises very greatly, only to fall off abruptly with further additions of either of these metals. Dr. Waldo : My curve related only to electrical conductivity. The President : If irregularity in one physical property argues

Jan 1, 1895

By John Birkinbine

Among the notable deposits of iron-ore, the Iron Mountain at Durango, Mexico, is prominent. But, although it has been noticed in records of travel and official reports for three centuries, the statements made concerning it have been so largely alloyed with improbabilities that general credence has not been given to data relating to the Cerro & Mercado, that being the name by which this remarkable mountain of ore is known. Location. Geographically, the mountain is centrally located, being situated immediately at the City of Durango, which is distant in direct lines (as the crow flies) as follows: From the Rio Grande River at El Paso, Texas, in the north, 510 miles; from the same stream at Laredo, Texas, in the northeast, 410 miles; from Tampico, in the east, 475 miles; from the City of Mexico in the southeast, 520 miles; from Mazatlan in the west, 110 miles. At El Paso, the standard-gauge Mexican Central Railroad, and at Laredo, the narrow-gauge Mexican National Railroad, enter Mexico. Tampico is a prominent Mexican port on the Gulf of Mexico, and Mazatlan occupies a similar position on the Gulf of California. To reach Durango from Laredo or Tampico, spurs of the Sierra Madre Mountains must be crossed, and between Mazatlan

Jan 1, 1885

By B. C. Allen

Surface free energy and surface self-diffusion of solid molybdenum were studied in the temperature range 1600" to 2400°C using pressure-sintered bi-crystals. Comparison of groove angles formed in various surfaces perpendicular to the grain boundary indicate a maximum of 1 pct variation in surface free energy with crystallographic mientation. This anisotropy tends to decrease with increasing temperature. The surface diffusion of the bicrystals is equivalent to that of sheet with a mild (100) Preferred orientation. Anomalously low values found for bi-crystals with surface orientations of (OOl), (012), and (011) are rationalized in terms of anisotropy in surface free energy. THE effect of crystallographic orientation on surface free energy1,' and surface self-diffusion3,4 has been primarily studied in fcc metals. The object of this work was to study the effect of orientation on surface diffusion and surface free energy of bcc molybdenum using pressure-sintered bicrystals. EXPERIMENTAL WORK Materials and Crystal Preparation. Arc-melted molybdenum rod was obtained commercially and electron beam zone refined at 50 cm per hr at 10- 5 torr to form single crystals about 8 cm long and 0.65 cm diam. Three crystals were prepared with axial orientations about 1 deg from [001.], [011], and. [111]. To reduce the carbon content, the crystals were annealed 2 hr in 1.4 atm flowing wet hydrogen at 2050°C. Then the oxygen content was reduced by annealing for 2 hr in -30°C dewpoint hydrogen at 2020°C. The resulting impurity analysis is given in Table I. Bicrystal Preparation. The single crystal rods were cut into transverse slices with a thin silicon carbide abrasive wheel to produce specimens about 0.6 cm long. They were mounted in epoxy and surrounded by stainless steel washers. Cutting in half was done longitudinally at various angles to known crystallographic planes containing the cylinder axis according to Fig. 1. To reduce surface deformation resulting from the cutoff wheel and thus reduce parasitic grain boundary formation on subsequent annealing, about 0.003 cm was manually ground off each cut surface with 600 grit paper. Care was taken to keep the surface flat. After removal from the mounts, one half was generally ro-tated 180 deg with respect to the other to give a po- tential symmetrical tilt grain boundary between the two halves. In the other cases when low misorienta-tion angles were desired, the crystals were not rotated. On the basis of symmetry, sufficient bicrystals were prepared to cover the entire range of misorientations for symmetrical tilt boundaries. The misorientations, +, ranged from 0 to 45, 0 to 90, and 0 to 60 deg for [001], [011], and [111] bicrystals, respectively. One [Ill] twist bicrystal was prepared from 2 single crystal discs rotated 17 deg relative to each other. Each specimen consisted of two pieces which were placed in a cylindrical tantalum can. Sharp edges were rounded and the fit was made as snug as possible to reduce subsequent deformation during bonding. The assembly and crystals generally were vicuum outgassed at 900" or 1700°C and then electron beam welded in the can at l x 10-4 torr. After being leak checked, the samples were placed in an autoclave and hydrostatically gas-pressure bonded5 in four batches under helium at 10,000 to 18,000 psi at 1650°C for 3 hr. Satisfactory bonds were obtained in many cases, and most of the crystals bonded after two exposures. The results did not appear to be affected by the various pressures used, preannealing conditions, crystal orientation, or time-pressure-temperature route taken to the final bonding condition. After bonding, the tantalum cans were selectively removed in cold concentrated HF. Measurements indicated overall deformation was under 1 pct. The bicrystals were metallographically ground and polished flat and perpendicular to the axis. Examination showed the boundaries were straight and almost free of parasitic grains caused by extraneous local deformation. Annealing. In preparation for thermal grooving, the bicrystals were cleaned and annealed by outgassing at 10-5 torr at 1900°C and heating at 2300°C under 1 atm 99.996 Ar for 0.5 hr. The crystals were held in a closed 4-deck box made of molybdenum sheet, and were heated in a Ta-1OW resistance furnace. The ar-

Jan 1, 1970

By J. Chipman, N. J. Grant, E. C. Roberts

An equilibrium study was made of the distribution of chromium and oxygen between liquid iron, containing less than 1 pct Cr, and simple slags of the CaO(MgO)-Si02-FeO-Cr& type in the temperature range 1526' to 1734OC. The effects of slag oxidation, temperature, and basicity were observed. IN spite of the fact that chromium is one of the most important alloying elements in steel, and exists in almost all steels as a significant residual element, little research has been done to determine its behavior in basic steelmaking processes. Considerably more work has been done under silica-saturated acid slag conditions. Korber and Oelsen,' Herasymenko,' and others have generally agreed that in acid steelmaking practice the chromium in the slag behaved as if it were present as the chrom-ous ion (CrO). Work by Hilty- ir, high chromium slags also indicated that chromium may exist as CrO. In basic slag systems no equilibrium data exist. Based on individual studies of basic open hearth and electric furnace practice, Bardenheuer," Rock-rohr,% nd HauckQ oncluded that: 1—chromium recovery increased with decreasing basicity, and 2— chromium recovery increased with increasing temperature, although the effect was small. In similar studies Yavioskii and Dzemyen' concluded that: 1— slag FeO is the most important variable, 2—the basicity of the slag has no effect on chromium recovery, and 3—slag viscosity is not high even when 20 pct Cr,O, is present. Lapitskii\ oncluded that chromium recovery improved as the basicity of the slag decreased and increased with increasing manganese in the metal. Regarding the effectiveness of CrZ08 as a base or acid in basic slags, both Kristofferseno and Trojer" reported that Cr,08 was an acidic component requiring neutralization as 2CaO-Cr,O,. Experimental Procedure The experimental apparatus and procedure used for the present research were similar in most details to those used by Winkler and Chipman" and were described in detail by them. A magnesia crucible was used, holding 60 to 80 lb of Armco iron which was decarburized with hydrogen to about 0.010 pct C. Since all the metal samples solidified without gas evolution, this carbon level was assumed not to be significant. Synthetic slags made by mixing pure oxides were used throughout the study. Temperatures were measured by means of calibrated W-Mo thermocouples and were checked by Pt-Pt-Rh thermocouples. The range of temperatures covered in this study was from 1526" to 1734°C. The chromium content of the iron was in the range 0.032 to 0.82 pct, although the bulk of the tests showed 0.04 to 0.2 pct. The slags were of the CaO(MgO)-SiO,-FeO-Cr,O, type in which the Cr,O, content was from about 2 to 20 pct, although most of the slags showed from about 2 to 10 pct. The FeO range was from about 10 to 65 pct. CaO and SiO, were in the range of about 5 to 45 pct each, yielding a rather wide range of basicity values. The first 12 heats were made without a sulphur addition, and with only 30 min allowed for slag-metal equilibrium to be reached. In previous research it had been shown that less than 30 min was adequate to achieve equilibrium in slags free of Cr2O8.11,14.15 A study of the present data indicated that some of the tests may not have reached equilibrium in this time; accordingly four additional heats were made in which at least 1 hr was permitted for equilibrium to be reached. For reaching

Jan 1, 1955