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By M. C. LYNN

RECENT completion of a $40,000 lubricating oil plant will make it possible for students in the School of Petroleum Engineering at the University of Oklahoma to carry out on a large scale the entire process of refining crude oil, from the time it is received in tank cars and pumped through the 1/4-mile University pipe line to storage tanks on the campus until the various products appear in finished form. This plant is part of a $100,000 expansion program which this school has been carrying out during the past year. Two years ago the Oklahoma State Legislature appropriated $50,000 for the School to use in improving its laboratory facilities. A few months later a $30,000 PWA grant was ob-

Jan 1, 1937

By R. F. Mehl

Jan 1, 1961

By James C. Word, R. M. McLouski

This paper will describe the development and application of large-scale integration techniques employed in the fabrication of a germanium multielement array. The array consists of 100 by 228 PNP bipolar transistors fabricated on 5 mi1 centers. Back-biased p-n junction techniques are used for electrical isolation of the individual elements. The end use of the array is a high resolution, large area IR sensor. The monolithic array is fabricated in 1 ohm-cm p-type germanium epitaxially deposited on 6 ohm-cm n-type substrate. Epitaxy was accomplished through the hydrogen reduction of germanium te trachloride. Di-borane was used as the dopant. Base regions are achieved by the diffusion of arsenic from doped oxide or arsine sources. Oxide-masking of the arsenic im-pzlvity was achieved by the chemical deposition of a boron doped glass. The emitter is formed by an aluminum alloy diffusion technique. Vacuum deposited aluminum is used for the emitter, interconnections, and for the contact and bonding pads. ALTHOUGH a great volume of literature pertaining to the development of large scale integration techniques (LSI) has been published for silicon and in particular silicon imaging applications,' to date only a small number of similar devices have been constructed using germanium technology.' Since the physical and chemical properties of germanium are vastly different from those of silicon, the fabrication technology for integrated structures in germanium is also different from that of silicon. In particular germanium does not possess a stable oxide as can be grown on silicon by heating in an oxidizing ambient for masking of dopants and passivation. This paper describes the application of germanium LSI techniques employed in the fabrication of a multielement infrared sensor array. The array is used in a high resolution, large area infrared sensor for operation in the 0.8- to 1.5-u spectral range. Back biased p-n junction techniques are used for electrical isolation of individual elements. Discrete germanium devices have been fabricated routinely for some time. However, mainly due to the lack of a suitable mask for selective doping and the high current leakages inherent in germanium p-n isolation, few monolithic germanium structures have been constructed. THE INFRARED MOSAIC A cross-sectional view of the array is shown in Fig. 1. The monolithic structure consists of 12,800 PNP transistor elements in a 100 by 128 matrix fab- ricated on 5 mil centers. The emitters of each line of transistors are connected together using aluminum interconnects while the strip collectors are connected together in series at right angles to the emitter lines. The selection of this structure is dictated by the readout technique involved. Access to each element transistor is obtained by applying a bias voltage to a particular collector strip and separately interrogating each emitter row. A charge storage, i.e., an integration mode is used for reading out this particular array Construction techniques available for use with germanium do not include a selective p-type diffusion capability for surface concentrations greater than 10" per cu cm and junction depths greater than about 10 u. This fact limits the type of structure that may be used. Therefore, an array of PNP transistors that did not employ p-type diffusions was chosen. The structure was fabricated by growing a 1 ohm-cm p-type epitaxial layer on a carefully prepared 6 ohm-cm n-type substrate. N-type dopants were used for the isolation and base diffusions and alloyed aluminum was used to form the emitter junctions. The array was then completed by evaporation of aluminum interconnections and contact pads. SUBSTRATE AND SUBSTRATE PREPARATION Germanium substrates of (111) orientation grown by both Czochralski and zone leveling techniques were utilized for mosaic fabrication. Czochralski substrates were preferred because of the lower dislocation densities available in this type of material. Dislocation densities for the Czochralski material were typically less than 3000 per sq cm, while those for the zone leveled material were typically less than 5000 per sq cm. All substrates were uncompensated to minimize thermal conversion problems in subsequent epitaxial and diffusion processing. Both in-house and vendor polished wafers were used. The in-house polishing technique employed consisted of an initial gross chemical etch in CP4 to remove saw damage from both surfaces. This was followed by a chemical-mechanical polishing operation of one side of the wafer. The chemical-mechanical polishing solution used was Lustrox 1000 (Tizon Chemical Co.), and consists of zirconium dioxide, sodium hypochlorite, water and a surfactant. The wafer thickness before and after polishing was typically 0.020 and 0.010 in, respectively. THERMAL CONVERSION The problem of thermal conversion of both the substrate and epitaxial layer was particularly acute because of the relatively low carrier concentrations employed in both regions. This problem has been encountered by other workers in the past.3 Without special treatment before epitaxial growth substrate conversion (n-type to p-type) and changes in the re-

Jan 1, 1970

Meeting of Jan. 23, 1914.-The President reported the appointment of Arthur S. Dwight and E. Gybbon Spilsbury as tellers to canvass the votes for the Annual Election of Directors. The President reported the appointment of the Committee on Precious and Base Metals, reorganized in accordance with the list on page xlvi. . The Treasurer was authorized to invest the sum of approximately $1,000, accruing from the sale of Life Memberships during the past year, by the purchase of one gold bond of the Interborough Rapid Transit Co., due 1966, at 5 per cent. The By-Laws of the San Francisco Local Section were approved. The recommendation of the Lord Kelvin Memorial Fund Committee that the balance of the fund unexpended be applied to the establishment of a Kelvin Gold Medal was approved. Forty-two members who had paid up all arrears of clues were reinstated. The sum of $100 was appropriated to the Columbia Local Section. The price of each of the three Volumes of Transactions of the year 1913 was established as $5 in paper and $6 in half-morocco. Forty-three Members, One Associate and four Junior Members were elected to membership in their respective classes.

Jan 2, 1914

[NORTH AMERICA UNITED STATES ALABAMA Birmingham CORD, Richard H DISMUKES, Edward B Citronelle PERRIN, Huey P Fairfield PAGEL, Herbert Ervin Huntsville ENG, Harvard KELLEY, Dean W WAGGONER, J B Mobile HORNER, William L PETROUTSON, Peter C Montgomery GAMBLE, Halbert R Redstone RAWLINGS, William E Tuscaloosa MASON, William L University CUDWORTH, James R JONES, Walter B]

Jan 1, 1961

By E. A. Calnan, B. E. Williams

IN the development of a new treatment for the prediction of deformation textures,'-' it was noted that for no metals are there experimentally determined tension textures with which the predictions may be compared. There is a considerable knowledge of drawing textures and previous workers have been content to consider these as equivalent to tension textures for the purposes of comparison. It is shown, however, in the new treatment that the tension and drawing textures are not necessarily identical, the radial compression exerted by the dies in the drawing operation producing some modification of the tension texture. In particular for the face-centered cubic metals it is predicted that for drawing the final texture should be [1ll] with a spread towards [211] (a more detailed derivation of this texture has been made by Calnan3). This has been amply confirmed by experiment, see Hibbard.6 For the pure tension case, however, the treatment predicts intermediate [1ll] and [loo] textures leading to a [211] end-point, while all previous treatments have predicted the final texture as [1ll] with in some cases an additional [loo] component. Thus evidence that the pure tension end-point is the [211], or at least that [1ll] and [l00] are not the final textures, should provide a valuable test of the new treatment. Accordingly some experiments were made on aluminum. Three aluminum specimens were examined in detail, one of cold-rolled high purity rod (99.99 pct), specimen A, and two of commercial extruded rod of purity 99.4 pct, specimens B and C. The initial annealing treatments were: A, 1½ hr at 400°C; B, 2 hr at 400°C; C, 1½ hr at 650°C. The principal difficulty is that of obtaining sufficient elongation before fracture occurs. This was overcome to some extent by giving a softening heat treatment, 1 hr at 300°C, after each 15 pct of extension. Vickers hardness measurements gave values before and after the softening treatment of about 30 and 28, respectively, in comparison with the initial value of about 19 corresponding to fully annealed material. From recent observations in this laboratory it is concluded that this small recovery corresponds to a polygonization process rather than recrystallization proper and consequently the preferred orientation is unaffected. At the higher extensions, however, some slight necking of the specimens took place and it was necessary to turn them down to a uniform cross-section before

Jan 1, 1953

By A. Kenneth Schellinger, O. Cutler Shepard

INTRODUCTION OVERGRINDING, or the breaking of ore particles into sizes smaller than required for liberation, is a first-magnitude problem in grinding for concentration processes. The conventional ball mill-classifier circuit used in commercial grinding produces mineral particles that are all ground to pass an upper size limit, while the proportion of very fine sizes, or slimes, is uncontrolled. Calculations based on measurements made in commercial plants which were grinding ore for flotation concentration indicate that about 90 pct of the energy used in grinding is consumed in useless overgrinding.1 In addition to accounting for the consumption of a large amount of energy, overgrinding is detrimental to the flotation process. Overground slime coats larger particles and inhibits selective action by the flotation reagents on particles which by themselves could be separated very well. A further difficulty is that extremely finely ground minerals do not respond satisfactorily to flotation-collecting reagents, and both selection and recovery decrease markedly with particles finer than 5 to 10 microns.2 Conventional classifier-ball mill circuits inherently tend to overgrind the valuable minerals more than the gangue minerals because most valuable minerals are of higher density and are softer and more friable than the gangue minerals. The remedy to this situation would seem to be a separating mechanism which would separate free valuable mineral particles regardless of size and density considerations and a mechanism which would operate in the grinding mill so that valuable mineral grains would be removed from the grinding machine as soon as they are freed. A consideration of these ideas led the authors to the conception of a simultaneous grinding and flotation mechanism. So far as the authors are aware, such a machine has never been tried, even on a laboratory scale. DEVELOPMENT OF APPARATUS AND EXPERIMENTAL METHOD Apparatus development went through several stages before a really workable machine was devised. Work was started with a large cast-iron mortar 7 ½ in. in diameter and 8 in. deep. A cast-iron disk was mounted on the end of a vertical shaft so that it fitted loosely into the bottom of the mortar. On top of the disk four radial cleats ¼ in. high were bolted to agitate the ball charge as the disk, or impeller, rotated. The vertical shaft was driven at 100 rpm by a mechanism improvised from an old coffeemill type of grinder. A hole was drilled into the bottom of the mortar through which compressed air was introduced for frothing. In operation, weighed charges of ore which had been crushed to pass an 8-mesh screen were placed in the bowl along with water and suitable reagents. The impeller was then started and the compressed air turned on so that the ore was ground while being exposed to air bubbles. Mineralized froth was

Jan 1, 1947

By H. W. Miller, V. H. Wilhem

Although the year 1933 was a period of uncertainty, considerable new development was initiated, with a high percentage of favorable results, for owing to financial conditions only projects of merit were proposed and developed. Unfavorable marketing conditions caused severe financial losses to refinery and sales departments of nearly all companies during the first half of the year. In anticipation of stabilized Government control, earnings were generally favorable during the third quarter but failure of the Government to take legal action against violators of the proration orders, and lack of agreement on a definite plan of curtailment, resulted in considerable overproduction and demoralization of the market structure during most of the final quarter. However, toward the close of the year Government action against violators of the Oil Code had a tendency to decrease overproduction materially and give the market a firmer tone. As a whole, the price structure of crude oil was maintained at a high level during the year; in fact, at a much higher level than the price of refinery products warranted. At no time during the year was production within 10,000 bbl. daily of the state allotment, overproduction of crude reaching a peak of 70,000 bbl. on Sept. 7, average daily average for the year being about 27,000 barrels. Numerous plans for equitable curtailment were prepared and tested during the year, none of which fully solved the many and intricate problems faced by operators who were in most cases willing to curtail if they could feel that cooperation was being practiced by their neighbors. Outstanding events in California oildom during the period under discussion may be classified under the following headings: 1. New discoveries. (a) New development in proven areas. (b) Deeper zones in settled pools. 2. Unproductive wildcat operations. 3. Whipstocking practice and procedure. 4. Progress of unit and orderly plans of development.

Jan 1, 1934

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By Elwood G. Haney, R. N. Parkins

Stress corrosion cracking of two heats of 18 pct Ni maraging steel in rod form immersed in an aqueous solution of 0.6N NaCl at pH 2.2 has been studied on un-notched specimens stressed in a hard tensilf machite. Austenitizing temperature in the range 1830 to 1400 F has been shown to have a marked influence on the propensity to crack, the loulest austenitizing- temperature producing the greatest resistance to failure. In the nzosl susceptible conditions, the cracks followed the original austenile grain boundaries; but when tlze steels zcere heal treated to inproze their resistance to stress corrosion, the cracks becatne appreciably less branched and slzouqed significant tendencies to become trans granular. Electron metallography of the steels indicated the presence of snzall particles, possibly of titanium carbide, along- the prior austenite grain boundaries and these particles u:ere more readily detectable in the structures that were most susceptible to cracking. Crack propagation rates, which appeared to be dependent upon applied stress and structure, were usually in tlze reg-ion of 0.5 mm per hr and may, therefore, be e.xplained on tlze basis of a purely electrochetnical ,nechanism. However, there is some ezliderzce from fractography that crack extension may be assisted by ttlechanical processes. Anodic stit)zulation reduced the tiwe to fracture, although cathodic currents of small magnitudes delayed cracking-; further increase in cathodic current resulted in a sharp drop i,n fracture litne, possibly due to the onset of hydrogen ewbrittlement. THE use of the high strength maraging steels, with their attractive fracture toughness characteristics, is restricted because of their susceptibility to stress corrosion cracking in chloride solutions. Although this limitation has resulted in investigations of the stress corrosion susceptibilities of these steels, there have been few systematic studies aimed at defining the various parameters that determine the level of susceptibility. It is the case that the usual tests have been performed with the object of defining some stress or time limit, on unnotched or precracked specimens, within which failure was not observed,' but while such results may be of some use in design considerations, they are necessarily concerned only with the steels as they currently exist and not with their improvement to render them more resistant to stress corrosion failure. This omission may be considered unfortunate because the indications are that stress corrosion in maraging steels shows dependence on structure in following an intergranular path, and since experience with other systems of intergranular stress corrosion crack- ing is that susceptibility may be varied by modifying heat treatments, a similar effect may be expected with maraging steels. It is sometimes from such observations that a fuller understanding of the mechanism of stress corrosion crack propagation begins to emerge, leading in time to the development of more resistant grades of material. The present work was undertaken to study only one aspect of the influence of heat treatment upon the cracking propensities of the 18 pct Ni maraging steel, namely the effect of austenitizing temperature, although certain ancillary measurements and experiments have been undertaken. EXPERIMENTAL TECHNIQUES Most of the measurements were made on a steel, A, having the analysis shown below, although a few results were obtained on a steel, B, having a slightly different composition. Both steels were supplied in the austenitized condition, A as 3/8-in-diam rod and B as 1/2-in.-diam rod. Cylindrical tensile test pieces were machined from the rods: the overal length was 2 1/2 in., the gage length 1 in. and the diameter 0.128 to 0.136 in. The stress corrosion tests were carried out with the specimens strained in tension in a hard beam testing machine, the necessary total strain being applied to the specimen over a period of about 30 sec, after which the moving crosshead was locked in position and the load allowed to relax as crack propagation proceeded; the load relaxation was recorded. The load was applied after the specimen had been brought into contact with the corrosive solution, the latter being contained in a polyethylene dish having a central hole through which the specimen passed, leakage being prevented by the application of a film of rubber cement. The specimen was in contact with the solution for over half of its gage length and the solution was exposed to the air during testing. The solution was prepared from distilled and deionized water to which NaCl was added, 0.6N, and the pH adjusted to 2.2 by HCl additions. The composition of the solution

Jan 1, 1969

By Haakon Styri

In discussion of Dr. Fitterer's paper on electrolytic separation of slag inclusions, some results from experiments on electrolyzing high-carbon steels at the SKF Research Laboratory were given. l We had been working for a number of years on chemical methods of separating the inclusions but could not find any solvent that would dissolve the steel without attacking some of the inclusions, particularly the sulfides in which we were mostly interested at the time, nor any that would dissolve all sulfide or silica in filings as fine as 300 mesh without attacking the iron. Electrolytic methods had also been tried without any real progress until we learned from the Bureau of Mines about the use of the collodion membrane around the anode. Our early difficulties were to some extent different from those of the Bureau of Mines, perhaps because of experimenting on steels of higher carbon content, but most of our difficulties were of the same nature as those of the Bureau. Formation of large quantities of basic hydroxides was traced to the use of impure and oxidized ferrous sulfate. To protect from oxidation from the atmosphere during electrolysis, after purer chemicals were obtained, a thin layer, 54 in. or less, of molten paraffin was poured over the surface of the cathode liquid, where it solidified. It was found desirable also to hold the cathode chamber slightly acid by initial addition of 0.1 per cent acid (sulfuric or hydrochloric) to prevent precipitation of the hydroxide. This acidity would decrease gradually and the cathode chamber would become neutral before the end of the electrolyzing. The increase in acidity in the anode chamber during our early experiments had appeared to cause attack of the precipitated sulfides in the residue, which originally was analyzed by volumetric method for sulfur, and for this reason a 10 per cent sodium citrate solution was substituted for the sulfate in the anode chamber. With the use of the more reliable Eschka method for sulfur determination (as in coke), there was however no serious attack on the sulfides in the anode chamber with a variety of different liquids, as shown in Tables 2 and 4. The Eschka method gives a higher sulfur value than

Jan 1, 1933

Discussion of the paper of F. C. LANGENBERG and R. G. WEBBER, presented at the New York meeting, February, 1915, and printed in Bulletin No. 98, February, 1915, pp. 291 to 300. HENRY M. HOWE, Bedford Hills, N. Y.-The results here given are of great interest and are welcome as forming another rivet to increase the stability of our present theories of the constitution and properties of steel. The important discovery is that the hysteresis increases with the fineness of the structure, that is to say with the extent of contact between the particles of ferrite and cementite. All of the specimens except No. 4 consist of ferrite and cementite of different degrees of intimacy of admixture. If hysteresis represents something akin to surface friction, which retards the rotation of the ferrite on the application and release of the magnetizing force, then it is only natural that it should increase as it does with the intimacy of admixture, because it is at the surface of contact of a given particle of ferrite with the neighboring particles of cementite that this friction is to be expected, and of course the extent of surface must in¬crease with the intimacy of admixture. The somewhat greater hardness of specimen 4 than of the others may perhaps he referred to the principle discussed in my paper, Why Does Lag Increase with the Temperature from Which Cooling Starts?' The furnace-cooled specimens were cooled so slowly that the influence of the initial temperature of heating is effaced. But in the air-cooled specimens we have the suggestion that the high temperature, 1,000°, from which the cooling of No. 4 started has prevented the completion of the transformation, with the result that the metal is slightly harder than any of the others. The difference is not to be explained by difference in the fineness of structure, because the whole range of fineness from No. 1 to No. 6 is accompanied by no change in hardness, the only change being an appreciable increase of hardness following the air cooling from 1,000°.

Jan 5, 1915

By Raymond C. Johnson

GASIFICATION is important to the anthracite industry, as it is to the entire solid-fuel industry and to the nation. However, to the anthracite industry it may have particular significance in that it would increase the market value of many millions of tons of a by-product fuel, which the industry now has in storage and is currently producing, in addition to increasing the potential market for all its products. The by-product fuel is of usable quality but the ash content is higher than it can be in other products and therefore it must be converted or used at the point of production. Gasification is one method by which the product may be given increased value. The inherent characteristics of anthracite make it well suited for producing a fuel or synthesis gas. It is the most concentrated form of natural commercial carbon, noncaking and noncoking; it does not produce smoke, tar, or soot and has a low sulphur content; and the volatile matter, which ranges between 2 and 8 pct, is 80 to 85 pct hydrogen with small amounts of methane, carbon dioxide, carbon monoxide, and nitrogen. The ash fuses at high temperatures, which allows it to be burned at high rates without slagging. However, with the addition of small amounts of dolomite, the ash will form a slag, or glass, which is very fluid. Anthracite has long been used in the manufacture of city gas and it is extensively used in various parts of the country to make water gas to be converted to hydrogen. Buckwheat and rice anthracite are used in Galusha producers to make producer gas. Excellent synthesis gas has been made in a Galusha producer with rice and barley anthracite with oxygen in tests at the Consolidated Mining and Smelting Co., Trail, British Columbia. In these tests, anthracite was shown to have advantages over competitive fuels, in that the gas had a higher hydrogen content and could be cleaned with less difficulty. The anthracite seams are steeply pitching and in mining the parting strata and some of the roof and bottom materials are taken with the coal. In preparation, these materials are separated by gravity from the commercial product and stored in refuse banks. This refuse contains a mixture of rock, slate, or shale, and high-ash anthracite with bone coal, which is low-ash coal that is interspersed with thin bands of shale. The bone coal contains between 25 and 50 pct ash with an average ash content of approximately 30 pct, with a

Jan 1, 1953

By Will Mitchell, T. G. Kirkland, C. L. Sollenberger

R. S. Handy (Santa Rosa, Calif.)—It would be interesting to learn the comparative results of treating the Korean scheelite ore described in this paper according to the following procedure: I—Follow the procedure described in the paper to the recovery of the sulphides by flotation. 2—Dilute the residue from the sulphide flotation strongly with water and disperse the contained colloids by adding a mixture of 75 pct sodium silicate and 25 pct quebracho to dispersion point. 3— Settle the dispersed pulp and decant the supernatant colloids. 4—-Dilute, settle, and decant the pulp until the settled residue is crystalline. Not over 10 pct of the tungsten minerals should follow the colloids. 5—Treat the settled residue by flotation, having established the proper pH. Oleic acid homogenized with cresylic acid or kerosene is more selective for scheelite than is oleic acid alone. (The recovery of the contained tungsten minerals should be practically complete in this operation.) 6—Deflocculate the tungsten concentrate from step 5 with the same dispersion agents as in step 2 and treat the deflocculated pulp by gravity. The minerals that tend to float with scheelite are generally of low specific gravity and the separation is efficient. The heavier contaminants, such as pyrrhotite and magnetite can be removed magnetically, leaving a practically pure scheelite. E. J. Pryor (Imperial College of Science and Technology, London)—It occurred to me that instead of using temperature as a differentiating control, more precision might be obtained with a reagent of a type we developed here for the flotation of high grade fluorspar in cold pulps. This reagent, which is manufactured on a modest scale in England, is based on oleic acid, which has been modified by our patented process to ensure complete stable dispersion at any desired concentration in water. It thus becomes possible to utilise unimolecular layers with good selectivity. In the fluorspar flotation for which we developed it, it is possible to hold a tight control on depressing quebracho for the calcite without substantial loss of flu-orite, and recovery exceeding 99 pct is not uncommon in the mill where it is in use, even under wintry conditions. No attempt has been made yet to extend the use of the reagent, as we have not completely overcome

Jan 1, 1952

By D. J. Jr. McAdam

Fort the past five years, an investigation of the endurance properties of metals has been in progress at the U. S. Naval Engineering Experiment Station, Annapolis, Md. As a result of the investigations at this Station1-5 and other laboratories6-11 "endurance limits" of practically all kinds of carbon and alloy steels have been determined and have been correlated with other physical properties, especially with tensile strength. About a year and a half ago, the investigation at the Naval Experiment Station was shifted to non-ferrous metals. As a result, several papers discussing the endurance properties of numerous non-ferrous metals and alloys, especially the alloys of nickel and of copper12-16 have been published. In these papers, stress-cycle graphs illustrate. the endurance properties of each individual metal and alloy, and other graphs illustrate the effect of cold working, heat treatment, and chemical composition on endurance and other physical properties. Endurance tests of non-ferrous metals were made by the machines used in the endurance tests of ferrous metals. 1-4 The specimen for the rotating-cantilever tests, which has been described, 1,2,13 has a conical surface, with taper so adjusted that the stress is nearly uniform over a length of about 1 ½ in. Alternating torsion tests were made with the machine of the inertia types17 and usually by an accelerated-fatigue method.12 As the rotating-cantilever endurance limits of metals are about twice the alternating-torsion endurance limits, the former values are more generally useful in correlating the endurance properties of nonferrous metals. In several recent papers by the writer13-16 correlation of the endurance properties of a number of non-ferrous metals has been discussed.

Jan 10, 1925

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,' there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells' and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported' in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F' (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 '/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By R. W. Bartlett

Hydrometallurgical processes for copper flotation concentrates avoid the SO2 emission problems associated with smelting, but they require oxidation of copper to obtain solubilization during leaching. The resulting copper ions must be reduced to metal, which normally requires large amounts of energy or energy equivalent reagents such as hydrogen or iron. The conventional reduction method is electrowinning which is labor intensive and involves 35 to 40% of both the entire operating and capital cost of the better hydrometallurgical processes. There is considerable incentive to reduce the cost and energy required for producing copper ions from solution. Furthermore, it is thermodynamically possible to do this using sulfur contained in the concentrate itself. In fact, the thermodynamic potential of oxidizing sulfur from S+4 to the S+6 state is greater than required to reduce cupric ion to metallic copper.1 Realization of this potential in a practical process would significantly reduce the cost of hydrometallurgical processing of sulfide concentrates because sulfur would become a cost-free reducing agent. An apparently practical method is to use SO: and HSO3 ions, obtained by ammonia scrubbing of SO2 from a concentrate roaster gas, to reduce leached copper to metal in an autoclave. This reduction step is the Jumau 1907 A series of steps, including sulfite reduction, constituting a crude flowsheet was suggested by Parker in 1976.3 The present paper describes a detailed complete. sulfite process flowsheet based on materials and energy balances, discusses the chemistry, and discusses further work that is required to develop this process. Process materials, utilities costs, and energy requirements are projected to be unusually low because of the utilization of sulfur from the concentrate. Process Description The sulfite reduction process requires a copper concentrate containing approximately as much sulfur on a weight basis as copper. For those few concentrates that are deficient in sulfur, additional sulfur can generally be obtained by allowing more pyrite to float in the concentration process. The process steps, shown in [Fig. 1], are (1) a fluid bed roast of the concentrate, (2) a leach of the roaster calcine using recycled barren liquor from the reduction autoclave, (3) scrubbing of the SO2 gas with ammonium sulfite liquor to produce ammonium bisulfite, (4) reduction and precipitation of copper in an autoclave by combining part of the SO2 scrubber effluent (SO5

Jan 1, 1980

By O. A. Cheadle, F. E. Lane

ThE computer program for arbitrary crystal systems reported by Camp and Clum' has been modified to make it more convenient for hexagonal crystals. The program' uses the Miller indexes (hkl) which can be confusing for hexagonal crystals while the modified program uses the Miller-Bravais indexes with four axes; e.g., the angles between the (110) planes, Fig. 1, are 0 and 90 deg but in the (hkil) system the angles between the (1150) planes are 0 and 60 deg. If a Laue photograph is taken of a crystal oriented with the prismatic planes nearly parallel to the film then the spots on the stereo graphic projection will be from high-index planes. The probable positions of the low-index planes, e.g., (0001) plane, can only be obtained from the intersection of zones and this is not accurate to 1 or 2 deg. The number of planes considered by the program (card 1)' has to be limited to the ones of low index or the program time is excessive but a solution will not be obtained if one of the spots has an index that is not being considered. To overcome this problem the program1 was modified so that if no fit was obtained at *1 deg (card 3) of the tabulated angles then ±2 or ±3 deg was tried. If still no solution was obtained either due to one of the angles not being measured correctly to ±3 deg or because one of the spots was from a high-index plane, then the last spot was discounted and a fit tried for the remaining spots at i1 deg, and so forth. The minimum number of spots that the program will try to fit is five. If the limit on any individual index is 4 (card 1) and (h + k + l + 1) is six then twenty-three planes are considered and there are over 1000 interplanar angles. Many pairs of planes have very similar interplanar angles and with the errors previously mentioned the program will often produce several alternative solutions to a group of spots particularly at ±2 or ±3 deg. However without the program the alternative solutions would probably not have been found. If a large number of spots are used the number of possible fits is reduced. In the example shown in Fig. 2, if only spots which are on the film are used (case 1) the program gives six possible solutions, Table I. However if points 7 and 8 are also used (case 2) the program gives only one fit which also agrees with a standard projection of the crystal. In addition to time-saving the program ensures that a correct solution is obtained since it is unlikely that all the alternatives would have been gound manually; the first would probably be assumed to be the correct solution. The program has been used for zirconium crystals but is equally suitable for other hexagonal materials.

Jan 1, 1969

By M. R. Geer, H. F. Yancey, P. S. Jacobsen

Two growing problems confront the preparation engineer—still further restrictions on stream pollution and a greater proportion of fine coal as more and more continuous miners come into use. The de-watering screens, centrifuges, and settling ponds that sufficed a few years ago must often be supplemented by more effective equipment, and in some instances the finest solids are now being recovered by vacuum filtration, once considered too costly in many coal washeries. Unfortunately not all slurries can be readily filtered. Some are virtually unfilter-able, and others do not permit the high cake rates needed to hold costs within reason. Often, however, these difficult slurries can be rendered filterable by flocculation. Starch and lime have long increased settling rate in thickeners and can also aid filtration. More recently there have been other flocculants, primarily synthetic polymers or gums. Reports of their great effectiveness prompted the U. S. Bureau of Mines to test their use in filtration as part of its program on recovering and cleaning fine coal. The object of the present work was to compare some of the newer flocculants with starch and lime and to test the reaction of different types of slurries to flocculation. Three natural slurries, three synthetic coal-clay mixtures, and five flocculants were tested, all with a laboratory filter leaf. Slurries and Flocculants Tested: First of the slurries was the thickener feed from the washed coal section of the Michel colliery of Crow's Nest Pass Co. Ltd., Michel, B.C. As shown by the screen and ash analyses in Table I, practically all this slurry was finer than 28 mesh, and about half the solids were finer than 200. Substantially all material coarser than 200 mesh was clean coal, but the ash content of 20.7 pct in the finest size indicates a moderate amount of impurity. This coal is medium-volatile bituminous in rank. Slurry was also obtained from the Black Diamond washery of Palmer Coking Coal Co., King County, Wash. This underflow of a 1/2-mm vibrating slurry screen is a waste product discharged to a settling pond. As shown by the data in Table I it contained about 20 pct material finer than 200 mesh, which analyzed 77.5 pct ash, indicating a high proportion of clay. The coarser sizes were also high in ash content because of the presence of bone and shale. Black Diamond coal is on the dividing line between bituminous and subbituminous rank. The third slurry, from the washery of Roslyn-Cascade Coal Co. in Kittitas County, Wash., was the underflow of a battery of 8-in. cyclones that is wasted with the coarser refuse from the plant. In both size and ash content this slurry was similar to the Black Diamond, but since it was a cyclone-underflow product, the fraction finer than 200 mesh undoubtedly contained a much smaller proportion of finely divided clay than was present in the Black Diamond slurry. The Roslyn-Cascade coal is high-volatile A bituminous in rank. Initially the slurry samples were stored in the laboratory at a concentration of 40 pct solids. A progressive change in filtration and flocculation characteristics during storage was noted, however, presumably because of progressive disintegration of the clay. After careful testing demonstrated that the slurry solids could be dried and then repulped without changing the original filtration characteristics, this procedure was adopted. The flocculants used were Separan 2610, Kylo 27, Jaguar MD-A, Idaho potato starch, and lime. The lime was used as a slurry, the Separan 2610 as a 0.10 pct aqueous solution, and the other flocculants as 0.50 pct aqueous solutions. The starch was causti-cized with sodium hydroxide before use. As some of the flocculants are reported to deteriorate on storage, new batches of flocculants were prepared every two days. Test Procedure: Fig. 1 diagrams the filter leaf apparatus employed. This consists of a test leaf having an effective area of 0.10 sq ft., a 60°, 8 1/2-in. diam cone to hold the slurry sample, a variable-speed electric stirrer, vacuum gage, bleed line for controlling vacuum, filtrate flask, moisture trap, and vacuum pump. Two filter cloths were selected—Saran SA 603, a monofilament, coarse-weave cloth, and polyethylene PO-801 HF, a monofilament, fine-weave cloth. The Saran was selected to provide maximum cake rate without regard to clarity of filtrate and the polyethylene to provide the best quality of filtrate without regard to cake rate. The test charge for the filtering vessel consisted of 800 g of solids (previously soaked for 24 hr) and

Jan 1, 1960