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By G. H. Bishop

The kinetics of the inter granular penetration and embrittlement of [100] tilt boundaries in 99.998 pct pure nickel upon exposure to bismuth-rich Ni-Bi liquids have been determined in the temperature range from 700° to 900°C. The kinetics of penetration are parabolic in time at constant temperature over most of the temperature range. In a series of 43-deg bicrystals the rate of penetration is anisotropic with respect to the direction of penetration into the grain boundaries. In lower-angle bicrystals the penetration rate is isotropic. The rate of penetration decreases with tilt angle at 700°C. The activation energy for penetration in the 43-deg bicrystals is 42 kcal per g-atom independent of direction. It is concluded that the intergranular penetration and embrittlement in the presence of the liquid proceeds by a grain boundary diffusion process and not by the intrusion of a liquid film. This was confirmed by a determination that the kinetics of penetration and embrittlement were the same in the 43-deg bicrystals upon exposure to bismuth vapor under conditions such that no bulk liquid phase would be thermodynamically stable. WhEN solid metals are exposed to a corrosive liquid-metal environment, the grain boundaries are sites of preferential attack. Depending on the temperature, the composition of the liquid, and the composition, structure, and state of stress of the solid, a number of modes of attack are possible. This paper reports a study of the kinetics of intergranular penetration and embrittlement of high-purity nickel bicrystals upon exposure to bismuth which, together with an earlier study by Cheney, Hochgraf, and Spencer,&apos; demonstrates that there are at least two modes of intergranular attack possible in the Ni-Bi system. In the study by Cheney et al., columnar-grain specimens of 99.5 pct pure nickel were exposed to liquid bismuth presaturated with nickel in the temperature range 670" to 1050°C. They found that the majority of the boundaries, which were predominantely high-angle boundaries, were penetrated by capillary liquid films, the attack proceeding by a process which will be termed grain boundary wetting. This process occurs in a stress-free solid when twice the liquid-solid surface tension is less than the surface tension of the grain boundary,* i.e., when 2yLs < YGB In this case the penetration of the grain boundary by the liquid occurs at a relatively rapid rate, resulting in the severe embrittlement of a polycrystalline solid. Grain boundary wetting is a common mode of intergranular attack in systems in which the lower melting component is relatively insoluble in the solid, but the solid has an appreciable solubility in the liquid, for example, the Ni-Bi system, Fig. 1. In systems of this type at temperatures above the range of stability of any intermetallic phases, once the liquid is saturated with respect to the solid so that no gross solution occurs, chemical gradients are small, and surface tensions become major driving forces for attack, provided the solid is stress-free. The results of Cheney et al. appear to be typical of those encountered when grain boundary wetting occurs.&apos; Capillary films were observed in the boundaries after quenching from the exposure temperature. The mean depth of penetration increased linearly with time, and the activation energy for the process was found to be 22 kcal per g-atom. In a study of the Cu-Bi system Yukawa and sinott4 found that the depth of penetration of bismuth into high-purity copper bicrystals of orientations from 22 to 63 deg of tilt about (100) at 649°C ranged from 0.05 to 0.25 in. after a 12-hr anneal. This corresponds to a linear rate of 6 to 15 X 10~6 cm per sec. At the same reduced temperature of 0.68 the rate for the Ni-Bi system&apos; was 7 x lo-&apos; cm per sec. In another study of the Cu-Bi system, Scheil and schess15 determined the kinetics of grain boundary wetting in hot-worked commercial rod. While there were several complicating factors present in this study, there is general agreement with the above results. The kinetics of penetration were linear, the activation energy was 20 kcal per g-atom, and at 650°C the rate of wetting was 2 to 5 x 10-6 cm per sec. The rate of wetting in the A1-Ga system6 is somewhat

Jan 1, 1969

By K. A. Svanstrom, W. R. Opie

Problems associated with deposition of titanium infused chloride baths using TiCl4 as a feed material are reviewed. A potentially workable cell design using Alumdum diaphragms is discussed. Problems inherent to diaphragm-type cells are emphasized and experiments described which led to the development of a cell without a diaphragm. INVESTIGATORS assigned the problem of developing a commercial electrolytic process for making titanium metal have found that they are faced with the difficulty of overtaking rapidly improving magnesium and -sodium reduction processes. The ultimate goal must be a simple process that can be conducted with low-cost raw materials in equipment that is inexpensive to build and operate. This paper deals with some work of a preliminary nature conducted by personnel of the Research Laboratories, National Lead Co., Titanium Division. Many others have reported on the general subject of depositing titanium from fused salt electrolytes. A partial bibliography is attached. PRIMARY CONCEPTS Anyone attempting to deposit titanium metal from fused chloride electrolytes using TiC14 as a source material is faced with at least the following problems: 1) Getting the titanium into solution in the bath. 2) Controlling oxidation and reduction reactions associated with multiple valency of titanium, which result in low electrical efficiency. a) Prevention of dichloride oxidizing to trichloride and trichloride to tetrachloride at the anode. b) Prevention of trichloride from being reduced only to dichloride at the cathode. 3) Prevention of metal formation away from the cathode thru disproportionation of titanium dichloride to satisfy the equilibrium. 3 TiCl2 == 2 TiCl3 Ti [I] 4) Protection of reduced chlorides in the bath from reaction with oxygen from the bath container or air. 5) Removing from the bath the deposited metal formed without allowing it to become contaminated with oxygen or nitrogen. 6) Selecting cell materials of construction which will not contaminate the metal product or cause cell inefficiencies. EARLY EXPERIMENTS The initial attempts made to electrodeposit titanium from fused chloride baths using TiCl4 as a source material indicated that TiCl4 was essentially insoluble in molten chlorides of alkali and alkaline earth metals. If, however, the TiCl4 was introduced close to a nickel cathode some metal could be formed and appreciable quantities of reduced chlorides would be present. These reduced chlorides reacted with any oxygen present in the atmosphere above the bath and would also diffuse quickly to the anode (graphite) where they would react with chlorine and be evolved as TiCl4. The net electrolytic efficiency of such a cell is essentially nil. The TiCl4 evolves from the anode at almost the same rate that it is introduced in the vicinity of the cathode although a small amount of titanium metal can be formed on the walls of the cathodic pipe. It becomes apparent from the operation of such a cell that: metal can be deposited on the cathode, although of small particle size and a nonadherent nature, and when reduced chlorides are present in the electrolyte, TiCl4 can be absorbed, probably by the following reactions: TiCl4 + TiC12 - 2 TiCl3 [21 2 TiCl3 + 2 faradays - 2 TiC12 + C12 [31 DIAPHRAGM CELLS These facts encouraged the development of cells containing diaphragms to prevent migration of reduced chlorides from the cathode area to the anode. Small-scale cells for process development are described by Alpert, Schultz, and Sullivan.20 A larger brick-lined cell incorporating internal heating by passing ac through the bath is shown in

Jan 1, 1960

By N. J. Grant, D. Carne, J. B. Seabrook

IT is unnecessary to review much of the literature on hydrogen embrittlement of steel since several excellent reviews and bibliographies exist.1-3 Hot acid pickling and cathodic charging have been known to cause hydrogen embrittlement of steel and have been used as laboratory methods to charge steels with hydrogen.4-8 Experimental Procedure The problem of prime concern in all instances, except in the work of Sims and coworkers,10 is that at no time was there a definite known hydrogen value reported which could be related to a particular value of the degree of embrittlement. It was the purpose of this research to determine the relationship between hydrogen content and degree of em-brittlement quantitatively. The 1020 stock used for the specimens was hot-rolled 7/16 in. diam rod of the following analysis: 0.19 pct C, 0.40 pct Mn, 0.012 pct P, 0.036 pct S&apos; Vacuum-fusion analyses for nitrogen and oxygen gave 0.014 pct O2 and 0.0011 pct N2. Cathodic charging was used to cause embrittle-ment. The advantages of this method were that no quenching was necessary, the impregnation was reasonably controllable, and representative samples for analysis could be prepared simultaneously with the charging of the tensile bars. Analyses for hydrogen were made in a vacuum-fusion type of apparatus which extracted gas from the samples by fusion in a molten tin-iron bath&apos; This apparatus, which has recently been described in detail elsewhere, will not be discussed here.". " Consecutive samples can be analyzed every 15 min with an accuracy of 0&apos;03 ppm. A A from an electrolytic or pickling bath can be charged for analysis in about 3 min, and analysis completed in 15 min. Samples of as-received 1020 stock were analyzed and found to contain a negligible amount of hydrogen (0.06 ppm). Preliminary pickling and electrolytic charging gave highly variable results. Cold-worked samples showed higher values but ranged from 0.6 to 6.0 ppm of hydrogen. Charging at 90°C gave higher values of charged hydrogen, but troublesome films on many of the specimens resulted. It was not until a few drops of a catalytic poison, prepared from 2 g of yellow phosphorus dissolved in 40 ml of carbon disulphide,8 was added to the electrolytic cell that fairly consistent high values of hydrogen could be charged into the as-received 1020 steel at room temperature. The cell used is sketched in fig. 1. The anode and fixture for the tensile specimens were fastened to the cell cover as shown, and the specimen was screwed in place, centrally located with respect to the anode. At first, anodes of lead and graphite were tried, but they contaminated the electrolyte and gave a slight deposit on the specimen. Later, a platinum wire was used in the form of a uniform helix. A current of 2 amp, corresponding to about 0.5 amp per sq in. of cathode, was used for most specimens. The electrolyte was 4 pct H2SO4 solution. Fig. 1 shows the form of the special tensile bar, the main portion of which was an ordinary 1/4 in. diam, 1 in. gauge length test bar, except that two to four small cylinders of stock were left attached by small links to the bottom end of the tensile bar for the purpose of providing samples for hydrogen analysis. Thus the bars and samples were charged with hydrogen simultaneously and an analysis could be made while the bar was being tested mechanically. Experiments were performed to determine how representative the test cylinders were of the middle of the test bar proper. While the bar center was being analyzed, the small cylinder was stored in dry ice, since it had been shown that such storage prevents loss of hydrogen for many hours.12 The results of these checks are shown in table 1. The checks are very good (0.3 ppm) and indicate that it is permissible to use the small end cylinders to establish the hydrogen content of the tensile test bar proper-

Jan 1, 1951

By N. Piret, B. Shoukry, S. Buntenbach

Traditional or artisanal goldmining, also known as small scale goldmining, has a strong and probably a negative environmental impact. The processing methods applied are very frequently a source of severe pollution due to the emissions of mercury by the extraction of gold by means of amalgamation as well as the emissions of cyanide through cyanide leaching of gold bearing ores. The emissions find their way into the environment and contaminate soils, sediments, water and atmosphere. Abnormal concentrations of mercury and cyanides in waterways are known to occur year after year destroying irreplaceable regions of the world. Mercury and cyanide compounds are highly toxic and may directly create permanent damage to the whole ecosystem. Existing methods for recycling of mercury and for decontamination of mercury and cyanide contaminated tailings are not customary applied in small scale mining and are ineffective as well. Based on investigations of traditional and small size goldmining, this paper presents: -processing methods of gold and discarded tailings under consideration of environmental protection; -figures on actual situation; -recommendations for equipment; -some decontamination methods for mercury and residual cyanide. Mineral Processing methods in traditional gold mining Gold is usually existing in its ores as the metal alloyed with metallic silver and perhaps copper. The element may occur in the form of: -native gold -inclusions also of microns or submicroscopic size metal sulfides (auriferous) such as pyrite, pyrrhotite, stibnite, arsenopyrite and galena -combined as telluride or sulphotelluride. The separation process selected depends on whether the gold can be freed from its unfavorable associations (e.g. gangue) at a sufficiently coarse grain-size, or whether it is carried in a heavy sulfide which can be freed similarly. The usual practice is to concentrate the goldbearing mineral at a relatively coarse grain-size and to regrind the ore if necessary. The gold content is concentrated by secondary or tertiary gravital methods or is extracted by chemical methods (amalgamation, cyanidation etc.) Gold, even when of fine grain-size, settle readily due to its high specific gravity from pulps in which the main gangue mineral is quartz or silicates. Amalgamation is the process of separating gold and silver from their associated minerals by binding (entrapping) them into a mixture with mercury. The cyanide process is applied to separate gold or gold-bearing compounds by dissolution from the finely ground ore (CIP, CIL, RIP), or as heap leaching. The dissolved gold is separated from the solids and the metal-rich or pregnant solution is then treated to recover its gold. Gold is also recovered by flotation methods. This process is widely used in treating base metal ores and in separating various sulfide components of ores, as well as in removing the barren gangue. The gold usually associates with a specific product in a sequence of flotation operations and is recovered subsequently in the smelting of the sulfide concentrates and refining of the metallic products, or by cyanidation of the roasted concentrates. Froth-flotation can be applied to separate gold and sulfide minerals from a finely ground pulp. The Amalgamation Process Amalgamation is the main method for the recovery of gold in traditional mining and is applied for the extraction of gold from placers as well as primary ores. The mineral technology used depends on the nature of ore deposits. In winning gold from solid ore, the matrix of minerals and rocks must be crushed and ground to sufficient fineness to liberate the gold. The liberated gold could be treated similar as free gold from placers. Gold is mainly separated from the valueless gangue (barren rock) by utilizing the difference between the density of the impure native metal (density about 16-19) and the gangue (density about 2.5). In simple operations the material is carried by a stream of water down a sluice generally equipped with small transverse barriers (riffles) against which the gold collects. The riffled sluice is the principal device used by artisanal gold miners. Nowadays, spirals as well as centrifuges, such as Knelson separator or Falcon separator, are occasionally applied for gold recovery. Gold may also be recovered from the pulp, by passing it over corduroycovered tables that catch the heavier particles - a method maybe as ancient as gold mining itself. In history, sheep skins were used to catch gold particles in this manner. Furtheron, gravity separation of gold is practiced on jigs, hydraulic traps, shaking tables and

Jan 1, 1995

By Kenneth P. Katen, Robert H. Trent

GENERAL DESCRIPTION Shortwall mining is one of the newest mining meth¬ods to be introduced into the world coal industry. The technique of shortwalling seems to have a number of origins, but it is generally agreed that it is an outgrowth of pillar-and-stall mining where timbering was employed as the primary means of roof support. In early opera¬tions the face was undercut by a shortwall cutter, hand¬bored, and blasted. The coal was loaded by hand or gathering arm loader. Australia, having experienced success with this method, advanced the technique through the use of mechanized roof supports in 1968. Although there were several attempts at shortwalling in the US, it was not until 1973 that Eastern Associated Coal Corp.&apos;s Federal No. 1 mine successfully extracted a shortwall panel. Table 1 is a list of shortwall opera¬tions in the US as of April 1976. Shortwall mining is a method of mining in which a continuous miner cuts and loads from the short end of a rectangular pillar of coal while hydraulically powered self-advancing roof supports provide protective cover. Characteristics of a shortwall system include panel di¬mensions (Fig. 1) of 610 to 1219 m (2000 to 4000 ft) in length, face widths of 30 to 61 m (100 to 200 ft), straight-line ventilation, and production machinery, with the exception of roof supports, commonly used on con¬tinuous miner units. GENERAL REQUIREMENTS AND LIMITATIONS The justification for shortwalling is primarily eco¬nomic, i.e., increased production and recovery concur¬rent with savings in material and labor. The method also has a number of secondary benefits including the much needed progress it has stimulated in deep mine technology, the alternatives it presents to some of the problems resulting from the 1969 Coal Mine Health and Safety Act, and is perhaps a key to the solution of the enigmatic labor problems which plague the industry. The advantages of shortwall mining over continuous miner units include the following: a highly effective method of ventilation and dust control; a greater per¬centage of extraction (approximately 85%) ; fewer equipment moves, hence more efficient operating time; cost savings on materials such as roof bolts, rock dust, ventilation curtains, timbering materials, and the labor needed to supply, load, and transport these materials; a cyclical pattern of mining, each phase of which, i.e., development and retreat, lasts for approximately three months and appears to be psychologically motivating as well as highly productive; and improved safety. In addition to these positive aspects, a shortwall sys¬tem also has advantages over a longwall system, and these are listed as follows: the capital outlay for a shortwall system is one-third to one-fourth that for a longwall (1976 prices); the shortwall system utilizes equipment that is used on a continuous miner section, with the ex¬ception of the roof support system; there is a great deal of flexibility in areas with numerous gas wells and in areas where surface subsidence cannot be tolerated; the shortwall has reduced tailgate problems, since the tail¬gate entry serves as a return airway only; and the cyclical pattern of mining insures that the mining machinery pro¬duces coal even while the roof support system is being moved to another panel. There are several parameters which govern the se¬lection and use of a shortwall system. They are all of equal importance, and hence are not listed in any par¬ticular order. These are deposit size, seam height, seam inclination, roof and floor conditions, depth of over¬burden, subsidence and chain pillar extraction, man¬power, ventilation, and materials handling. Deposit Size Reserves available for shortwalling should be suffi¬cient for at least an eight to ten-year period, since this seems to be the effective life, without rebuilding, of a hydraulic roof support under average conditions. Of

Jan 1, 1982

Fathi Habashi, Chalcopyrite. Its chemistry and metallurgy. New York, McGraw-Hill, 1978. 165 pp. RI9,95. Loss prevention and safety promotion The Proceedings of the 2nd International Symposium on Loss Prevention and Safety Promotion in the Process Industries, Heidelberg, 6th to 9th September, 1977, are now available. Chemical reaction engineering The Proceedings of the 4th International/6th European Symposium on Chemical Reaction Engineering (4th ISCRE) held at Heidelberg, Federal Republic of Ge rmany, from 6th to 8th April, 1976, are available from DECHEMA Deutsche Gesellschaft fur Chemisches Apparatewesen, P.O.B. 970146, D-6000 Frankfurt/ Main, West Germany, at the price of DMlOO plus postage and packing. Books received The Institution of Mechanical Engineers Proceedings Volume 190. Tribos abstracts on friction lubrication wear. Published by BHRA Fluid Engineering, Cranfield, Bedford MK 43 OAJ England. Price £30 (UK), US$72 (Europe), Seawater corrosion handbook, edited by M. M. Schumaker. Noyes Data Corporation Publicity Department, Mill Road at Grand Ave., Park Ridge, NJ 07656. 494 pp. Australian mineral industry quarterly 31(1) 1978 and 31(2) 1978. Bureau of Mineral Resources, Geology and Geophysics, Box 378, Canberra City, ACT 2601 Australia. Subscriptions $8, individual number $2. Mineral and NIM reports Report no. 1996 The extraction of gold from chloride solutions. (10th Nov., 1978). Report no. 1898 Batch and pilot-plant tests on M erensky Reef ore from the Western Platinum Mine. (8th Jun., 1977; reissued 30th Jan., 1979). Report no. 1920 A mineralogical investigation of Mamatu&apos;an and Wessels manganese ores. (15th Sep., 1977; reissued 3rd Jan., 1979). Report no. 1978 The preparation and certification of a referencesample of magnetite ore. (22nd Dec., 1978). Report no. 1998 Electrode response to the addition of zinc during the cementation of gold. (25th Jan., 1979). Report no. 2002 The spectrochemical determination of phosphorus, magnesium, and iron in phosphate rocks and sulphuric acid leach liquors. (26th January, 1979). Report no. 1992 The use of emission spectrometry for the determination of impurities in metals. (24th Jan., 1979). Report no. 2003 An electrodeless conductivity meter of improved sensitivity and reliability. (28th Feb., 1979). Report no. 2005 The spectrometric analysis of manganese-bearing materials with particular reference to ferromanganese slags and metals. (16th Mar., 1979). Report no. 2006 An examination of procedures for the analysis of dry powders by atomic-absorption spectrophotometry. (28th Feb., 1979). Report no. 2007 The instrumentation and computerization of a 25 MV.A submerged -arc furnace. (25th Mar., 1977; reissued 16th Mar., 1979). Corrosion The International Corrosion Council has decided to hold the next Internat ional Congress on Corrosion in Mainz, Federal Republic of Germany, from 6th to 11th September, 1981. Process control The First European Symposium on Real -time Datahandling and Process Control will be held in West Berlin from 23rd to 25th October, 1979. Geomechanics The 28th Geomechanics Colloquy, organized by the Oosterreichische Gesellschaft fur Geomechanik, is to be held at Salzburg on 18th and 19th October, 1979. Geosta tistics A short course on &apos;Geostatistics for exploration and production planning&apos; is being conducted by the Applied Earth Sciences Department, Stanford University, California, from 27th to 31st August, 1979. Business administration The Twelfth Executive Development Programme of the Graduate School of Business Administration, University of the Witwatersrand, is to be held from 9th July to 17th August, 1979. The engineer and the law A series of four meetings on the above subject is being conducted by the Measurement, Computation and Control SubCommittee of The South African Institute of Electrical Engineers. Lead smelter for South Africa? The National Institute for Metallurgy and Gold Fields of South Africa are making a comprehensive joint investigation of the technical and economic viability of an integrated lead smelter. Conference on titanium The Fourth International Conference on Titanium will be held from 19th to 22nd May, 1980, in Kyoto, Japan.

Jan 1, 1979

By E. G. Parker

"Sherritt&apos;s zinc pressure leaching process converts zinc sulphide concentrates directly to zinc sulphate solutions and elemental sulphur. Thus, one pressure process step replaces both the roasting and leaching operations of the conventional roast-leach route. In addition, high single-pass extractions eliminate the need for residue treatments to recover unleached zinc. Because pressure leaching produces elemental sulphur, rather than sulphur dioxide, acid plants and smoke stacks are not required, and air pollution control and work-place hygiene are greatly improved. .In 1977, Cominco Ltd. and Sherritt Gordon Mines Limited jointly operated a three-tonne-per-day pilot plant to demonstrate pressure oxidative leaching of Sullivan zinc concentrate and the subsequent separation of elemental sulphur. The process consisted of regrinding the concentrate, continuous leaching at 150°C at elevated oxygen pressures in a four compartment autoclave and the subsequent recovery of elemental sulphur, either in the molten liquid form from a decantation autoclave or as a flotation concentrate. Of the zinc contained in the concentrate, 97% was extracted in 90 minutes, and 96% of the sulphur was converted to the elemental form.Following the successful pilot campaign, Cominco began building the world&apos;s first commercial zinc pressure leaching plant. This plant, which was in operation by late 1980, will eventually treat about 25% of Cominco&apos;s planned zinc capacity of270,000 tonnes per year.This paper describes the general process principles, the results obtained from the pilot plant and the integration of the process into Cominco&apos;s operations at Trail. The application of pressure leaching to a ""grass-roots"" plant is also discussed, and compared with conventional roast-leaching."

Jan 1, 1981

By M. W. Bartley, Hugh M. Roberts

Substantial deposits of Bessemer hematite have been found recently by drilling beneath Steep Rock Lake, Ontario, which is situated in the northern part of the Lake Superior Region. It will be practicable to divert the waters flowing into this lake and develop open pits on the upper pert of two large ore bodies by damming off and pumping out the water in the part of the lake in which they occur. Ultimately, the bulk of the ore will be mined by underground methods. Owing to the generally massive nature of the rocks in the area, no underground flows of major consequence are anticipated after diversion of the lake. The Steep Rock deposits are attributed in origin to hydrothermal replacement. They were formed, for the most part, along an unconform-able, brecciated contact between the Steep Rock limestone and an overlying younger volcanic series, The replacing solutions came in as igneous after-effects, following upon the intrusion of basic igneous rocks that invaded the hanging-wall volcanics. It is believed that this took place in a geological period roughly equivalent to late Middle Huronian, which was the period when the most extensive iron-bearing rocks of the Lake Superior Region were formed. Comparison is made with other deep-seated iron-ore bodies in the Lake Superior Region, the origins of which are ascribed in the discussion to hydrothermal replacement. Introduction Under the waters of Steep Rock Lake, Ontario, situated on the Canadian National Railway, 142 miles west of Port Arthur, the presence of three ore zones containing red and brown Bessemer hematite has been established. These were discovered and have been partly explored by means of diamond and churn drilling, The positions of the ore zones, designated as A, B and C, are shown on the accompanying maps and cross sections. This exploratory work, begun in 1938 by Joseph Errington* and Julian G. Cross, has been carried on by Steep Rock Iron Mines Ltd., and was continued during the winter of 1941-1942. For more than 60 years explorers have known that large quantities of hard hema. tite float of good grade existed along the south shore of Steep Rock Lake, and the presence of ore beneath the lake was inferred by many early geologists and explorers. Despite numerous previous attempts to find ore in place, actual discovery awaited the recent period of intensive exploratory effort in Canada. The results obtained in the drill holes put down since 1938 by steep Rock Iron Mines Ltd. are not only of interest, in themselves, to those concerned with the development of ore deposits, but, taken in connection with the surface exposures of adjoining formations, they form the assemblage of facts from which the geological reasoning in this paper proceeds; accordingly, they are set out here as briefly and exactly as may be.

Jan 1, 1949

By M. W. Bartley, Hugh M. Roberts

Substantial deposits of Bessemer hematite have been found recently by drilling beneath Steep Rock Lake, Ontario, which is situated in the northern part of the Lake Superior Region. It will be practicable to divert the waters flowing into this lake and develop open pits on the upper pert of two large ore bodies by damming off and pumping out the water in the part of the lake in which they occur. Ultimately, the bulk of the ore will be mined by underground methods. Owing to the generally massive nature of the rocks in the area, no underground flows of major consequence are anticipated after diversion of the lake. The Steep Rock deposits are attributed in origin to hydrothermal replacement. They were formed, for the most part, along an unconform-able, brecciated contact between the Steep Rock limestone and an overlying younger volcanic series, The replacing solutions came in as igneous after-effects, following upon the intrusion of basic igneous rocks that invaded the hanging-wall volcanics. It is believed that this took place in a geological period roughly equivalent to late Middle Huronian, which was the period when the most extensive iron-bearing rocks of the Lake Superior Region were formed. Comparison is made with other deep-seated iron-ore bodies in the Lake Superior Region, the origins of which are ascribed in the discussion to hydrothermal replacement. Introduction Under the waters of Steep Rock Lake, Ontario, situated on the Canadian National Railway, 142 miles west of Port Arthur, the presence of three ore zones containing red and brown Bessemer hematite has been established. These were discovered and have been partly explored by means of diamond and churn drilling, The positions of the ore zones, designated as A, B and C, are shown on the accompanying maps and cross sections. This exploratory work, begun in 1938 by Joseph Errington* and Julian G. Cross, has been carried on by Steep Rock Iron Mines Ltd., and was continued during the winter of 1941-1942. For more than 60 years explorers have known that large quantities of hard hema. tite float of good grade existed along the south shore of Steep Rock Lake, and the presence of ore beneath the lake was inferred by many early geologists and explorers. Despite numerous previous attempts to find ore in place, actual discovery awaited the recent period of intensive exploratory effort in Canada. The results obtained in the drill holes put down since 1938 by steep Rock Iron Mines Ltd. are not only of interest, in themselves, to those concerned with the development of ore deposits, but, taken in connection with the surface exposures of adjoining formations, they form the assemblage of facts from which the geological reasoning in this paper proceeds; accordingly, they are set out here as briefly and exactly as may be.

Jan 1, 1949

By C. R. Sandberg, C. A. Connally, N. Stein

This paper describes the results of volumetric efficiency tests on oil well pumps handling gas oil mixtures. The work was performed in a large scale, above ground unit wherein test conditions could be accurately controlled and measured. The main variables studied were gas/oil ratio (including gas from solution and free gas mixed with oil), pump compression ratio, pump stroke length, pump speed, and clearance volume between the valves at their closest approach. Results are presented for two different pumps and for oils of two viscosities. Relatively small amounts of gas entering the pump resulted in large decreases in volumetric efficiency. Under conditions where the pump was operating at reduced efficiency because of the presence of gas, it was found that variation in the clearance volume between the standing and traveling valves had a considerable effect on pump efficiency level. This effect of the valve clearance volume was found to be significantly altered by the viscosity of the oil used in the tests. The effects on pump efficiency of the other variables studied were found to be relatively small over the range of conditions utilized. INTRODUCTION The production of oil by pumping is often hampered by low volumetric efficiency. A direct increase in lifting costs results from low volumetric efficiency. An indirect increase in lifting costs, probably greater than the direct increase, results from additional wear and tear on pumping equipment and from the down-time necessary for the repairs which can be traced to low-efficiency operation. Both increases in lifting costs tend to reduce economically recoverable oil. A number of different factors can contribute to low pump efficiency. A known basic cause of low efficiency is the presence of free gas in the pumped fluid. Pump volumetric efficiency is calculated only on the basis of liquid pumped and because any free gas pumped is discounted, this volume of free gas would represent a loss of pump efficiency. However, gas also causes a reduction in pump efficiency because it is a highly compressible fluid. It is known that pumps some- times "gas lock" because of excessive gas-to-liquid ratios in the pump barrel. Little is known of the role of gas compressibility in the intermediate case where the pump is operating at low efficiency. The opinion exists, however, that oil-well pumps tend to operate at higher efficiency with long stroke lengths at low speeds, but no quantitative studies of these pumping variables have been reported. It was believed that a much better understanding of the variables which control pump volumetric efficiency could be obtained and that possibly some suggestions as to the methods for increasing efficiency might be found from a study of the operation of pumps handling gas under closely controlled conditions. Previous investigators have studied the effects on pump efficiency of such factors as oil viscosity, oil temperature, slippage of oil. past pump plungers, pump submergence, valve size and spacing, pressure above pump plunger and fluid vapor pressure. However, none of these published investigations were conducted with pumps being subjected to large amounts of gas such as might be the case in a pumping well, nor did any of the investigations study the effect of variation in stroke length or pump speed. A large-scale teat unit was therefore constructed for studying the operation of pumps handling gas and for evaluating effects of such variables as pump stroke length and pump speed. PROCEDURE AND EQUIPMENT A schematic diagram of the pump testing equipment is given in Fig. 1. A 45-ft length of 6-in. casing is mounted vertically in a 65-ft tower. Sight ports are mounted in the casing at intervals near the location of the pump intake and the liquid level in the casing. These sight ports are fitted with Lucite windows sealed by neoprene "0" rings. The Lucite windows are machined to conform to the I.D. of the casing so that no obstruction to flow is present along the casing wall. The casing is fitted with a tubing head and 2-in. tubing is hung inside the casing. Pumps are seated in a shoe attached to the 2-in. tubing. A 1-in. polish rod is attacked directly to the pump without any intervening sucker rods. The top of the polish rod is attached to the weight carrier, which contains a number of weights to be used to force the polish rod in against tubing pressure on the down-stroke. This is necessary because a long string of sucker

Jan 1, 1953

By J. B. Newkirk, A. H. Geisler

The alloy Cu4Pd has a disordered face-centered-cubic structure when quenched from temperatures between 478ºC and the melting point (about 1100°C). Below 478ºC an ordered phase is stable. The results of a Debye-Scherrer X-ray analysis indicate that the ordered phase has a tetragonal unit cell described by the space group C24h — P42/mt with 2 Cu in 2a, 2 Cu in 2f, 4 Cu in 4j (x = 0.2, y = 0.6), 4Pd in 4j (x = 0.4, y = 0.2), and 8 Cu in 8k (x = 0.1, y = 0.3). The orientation relationship between the face-centered-cubic phase and the ordered tetragonal phase is given by: [100],,. // [130]al,. COO1Ia.d.//COO1I,,.. • The behavior of Cu,Pd is typical of ordering alloys except that the transformation is very sluggish. The increase in hardness and the microstructural and X-ray diffraction effects are interpreted in terms of coherency strains caused by the ordering. AN anomalous construction in the Cu-Pd phase diagram (Fig. 1) was reported in 1939 and has been allowed to stand without further published attention since that time. The odd figuration about the composition 10 to 27 atomic pct Pd is derived mostly from the work of Jones and Sykes.1 Evidently several features of this binary system require further study if the constitutional forms are to be well understood. The present paper includes a study of one of these features, that is, the crystal structure of a single ordered alloy containing nominally 20 atomic pct Pd. This choice of composition was suggested by the work of Harker and associates who determined the structure of Ni4Mo2 and Ni4W.3 The nature of the ordering process in Cu4Pd was studied also by observing the hardness, microstructure, and Debye-Scherrer patterns of specimens which had been aged at various temperatures after quenching from an initial disordering treatment. Experimental Methods A 20 gram ingot of Cu4Pd was made by melting spectrographically standardized copper from Johnson, Matthey, and Co., and commercially pure (99.5 + ) palladium in an argon-filled quartz tube. Chemical analysis showed that the ingot contained 80.0 atomic pct Cu. The ingot was rolled about 60 pct to a strip 0.060 in. thick and was homogenized for 16 hr at 950°C in low pressure argon. Rods cut from the rolled strip were worked into wire 0.015 in. in diameter, and specimens for hardness and microscopic examination were cut from the remaining strip. All specimens, with the exception of some of the wire, were given an initial disordering treatment by heating for 16 hr at 950°C, followed by water quenching. A 10 cm length of as-drawn wire was water quenched after being held in a temperature-gradient furnace4 for 89 days. Room-temperature Debye-Scherrer photograms were then made at points along the wire to determine the temperature below which the ordered phase was stable. Although the accuracy of temperature determination in the gradient was only about ±10 °C, the temperature gradient was sufficiently gradual that the sensitivity was much better and locations which had differed by as little as 1°C could be distinguished. An analysis of the crystal structure of the well ordered alloy was made by X-ray diffraction using a specimen cut from this wire. The change of Debye-Scherrer pattern as ordering progressed was studied by using isothermally aged samples of initially disordered wires. The wires were sealed under low-pressure argon in small quartz tubes for heat treatment. After the aging treatment, the tubes were quenched in water and photograms were made at room temperature in a 10 cm diam camera using filtered Cu kX. (A = 1.540511) Hardness was measured on a Vickers hardness tester using a 10 kg load and 2/3 in. objective lens. Reported values are the average of at least three impressions made on flat specimens 0.060 in. thick. After the hardness of a heat-treated sample had been measured, it was resealed in low-pressure argon and returned to the furnace for continued aging at the same temperature. In this way, two samples served for all aging times at each temperature. Hardness specimens which had been aged 500 hr or more were used for metallographic examination after the final aging treatment. A dilute potassium-dichromate etching solution was used.

Jan 1, 1955

By Charles Austin

IN an earlier series of studies on 18-8 stainless steel at 600°, 700°, and 800°C.1 one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manu-factured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in, dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0,07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recom-mended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 750°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8 -in. dia., air cooling followed the annealing treatment. These treatments per-mitted two direct comparisons: (1) between the 1150° and 950°C. treat-ments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950° and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By G. Gabra

"A process of leaching niobium oxide from pyrochlore concentrate using hydrofluoric acid is described. Variables such as acid concentration, temperature, reaction time, solid/acid ratio, agitation speed and particle size are correlated to the recovery of niobium oxide.The relatively low activation energy (1,86 Kcal/mole) and the dependence of reaction rate on agitation suggest that the process is diffusion controlled. The optimum conditions for extracting niobium oxide from the leach solution, using either methyl isobutyl ketone or tributyl phosphate have been determined.IntroductionMost of the commercial production of niobium and tantalum has been derived from the treatment of columbite - tantalite minerals.In recent years (1960) , pyrochlore mineral has been found to be an alternate source of niobium . This mineral varies widely in composition and contains in addition to the main elements of calcium , sodium and niobium, some tantalum, fluorine, rare earth elements, titanium, alkali an d alkaline earth elements.It is well known that the province of Quebec possesses several pyrochlore niobium deposits totalling approximately 151 million ton s at an average 0.45% niobium oxide(1). One of the deposits, the St-Honor carbonatite, was brought into production by Niobec Inc. in 1976. Flotation o f this material produces a concentrate of about 60% Nb205(2).In view of an expanding niobium market in recent years and the presence of large niobium deposits in the province, a research and development program was initiated at the Centre de Recherches Miner ales to evaluate known processes for the separation of niobium and tantalum from each other as well as their purification . Some work has also been undertaken at the CRM to develop an improved extraction process. T his work will be the subject of further communication s."

Jan 1, 1985

By Jancar T, de Guzman M M, Matthews B, Tu J. Y

The use of computational simulation to predict the performance of existing equipment or for the design of improved mineral processing equipment will be referred to as Computational Mineral Processing (CMP) in this paper. The emphasis will be on solving the governing equations for liquid solid flows in complex geometric domains to obtain, typically, the three-dimensional distributions of velocity and pressure for the liquid phase and the velocity and concentration for the solid phase. The underlying technology, computational fluid dynamics (CFD), is very well-developed in other industries (aircraft, car and chemical) and forms a vital part of product design and analysis. The subsequent design of improved mineral processing equipment may also involve finite element structural analysis (FESA). Computational fluid dynamics (CFD) and finite element structural analysis (FESA) are part of the generic discipline of Computational Engineering and Science (CES). Ciment and Scherlis (1993) define CES as `The systematic application of computing systems and computational solution techniques to mathematical models formulated to describe and simulate phenomena of scientific and engineering interest&apos;. Increasing computer power (Kaufmann and Smarr, 1993), is a dominant factor determining the rapid growth of industrial utilisation of CES. This increase is happening at both the supercomputer and the workstation level. Indeed, today&apos;s typical workstation, a Hewlett-Packard 735, is as powerful as a CDC 7600, the leading supercomputer in 1970. Future computer architectures are expected to become increasingly parallel (Gartner Group, 1990) allowing a sustained performance of a teraflop (a million megaflops) to be achieved well before the Sydney Olympics in the year 2000. It is recognised that the modem development of most disciplines in the physical sciences rests on the three complementary strategies of experimentation, analysis and computational simulation. As the 21st century is approached the volume of computational simulation, both fundamental and applied, is growing dramatically and the role of experimentation is diminishing. In the area of equipment design, CES provides the following advantages over experimental testing and measurement: 1. lead time in design and development is significantly reduced; 2. CES can simulate conditions not reproducible in experimental tests; 3. CES provides detailed and comprehensive information; and 4. CES is more cost-effective and time-efficient. The ultimate benefit for industry is greater productivity and hence greater profitability. The broader issues in relation to CFD are discussed by Fletcher (1993b). In the five- to ten-year time frame, growth in computer power will make it practical to combine CFD and FESA with optimisation procedures to produce a design process that is almost fully computerised. It is expected that fully automatic

Jan 1, 1995

By G. R. St. Pierre, L. M. Adelsberg, R. Speiser

The rate of scale fot&apos;~I~ti0n on tantalum held in H20-Hz-Ar gns mixtures at temperatures between 840" and 1250°C is related to gas composition and ternpevature. It is found that water vapor partial pressure determines the oxidation rate at a given temperature and that the oxygen potential as fixed by the water vapor to hydrogen ratio Ins no significant effect on the oxidation rate. The Ta205 scale formed during oxidation is composed of an inner lattice-dijf~ision barrier and an outer layer of- cracked/porous oxide 1 HE oxidation of tantalum at temperatures less than 800°C is characterized by solution of oxygen into the metal,&apos;-&apos; the formation and growth of suboxides into the metal,&apos;)2~10-15 and the delayed nucleation of the highest oxide, Above 800°C, Ta205 is found to nucleate rapidly10, 11, 15, 16 except at low oxygen pressures:15 however, there is uncertainty regarding which does not retard the oxidation process. For each gas con~position and temperature investigated, the oxidatioz rate becomes constant after a short adjustment period. It is shozm that a constant oxidation rate nzay pre~?ail even though the tlzickness of the inner lattice-dijjitsion layer of Ta205 is clanging. TFze initial czcrz!ature of the typical &apos;Paralinear" oxidation curve may result froprz causes other than an increasing thickness of tlze inner protective layer. the detailed mechanisms of the high-temperature oxidation. Peterson, Fassell, and wadsworth17 observed linear oxidation behavior for tantalum in oxygen at temperatures between 600" and 1000°C. They reported that equilibrium adsorption of 0, occurs on a surface prior to the rate-deter mining step of the reaction. Cowgill and stringer1&apos; confirmed the observations of Peterson and his coworkers. They stated that the rate-determining step of the reaction could be either the incorporation of adsorbed oxygen into the anion lattice or the dissociation of 0, at the gas-oxide interface. The relative rates of the two surface reactions were proposed to be dependent upon the reaction temperature and the oxygen pressure. stringerlo subsequently reported that the reaction surface is located somewhere

Jan 1, 1968

By A. Styka, G. Fischer, S. Tour

Described herein are the results obtained during research work involving coating titanium alloys with molybdenum by vapor-deposition methods. Results show that the method can be used successfully to deposit hard adherent wear-resistant coating of methodmetallic molybdenum on titanium or titanium alloys without changing the microstructure of the titanium base. PRODUCTION and use of titanium and its alloys have increased tremendously in the past few years. The physical, mechanical, and chemical properties of this engineering metal have caused considerable enthusiasm among metallurgists and engineers. However, as with all materials, there are some drawbacks. For example, titanium is susceptible to seizing and galling on wearing surfaces. In order to produce a good wear-resistant surface, many investigations have been conducted evaluating oxidizing, carburizing, nitriding, carbonitriding, sili-conizing, and chromizing of titanium. All of these processes require high temperatures for rather extensive periods of time. It has been possible to produce hard surfaces on titanium and its alloys by a number of these processes at the expense of a deterioration of the physical properties of the base material. A practical solution to the problem of providing titanium and titanium alloy parts with a satisfactory wear-resistant nongalling surface must be one that does not involve excessive temperatures for long periods of time. Sam Tour & Co. Inc. has completed a research and development contract for the United States Army Ordnance Corps on vapor deposition of molybdenum on titanium and titanium alloys. On the basis of results obtained from the research program, titanium alloys can be coated successfully with molybdenum to provide a hard wear-resistant surface without harm to their base mechanical properties. The remainder of this article is a description of the techniques used to apply the coating and the results obtained from wear tests on molybdenum-coated titanium. Theory Basically, the technique used was the application of molybdenum by a vapor-deposition method, thermal decomposition of molybdenum hexacarbonyl [Mo(CO)] with hydrogen as the carrier gas. The selection of this method was based chiefly on the following considerations: 1—low plating temperature which would minimize excessive grain growth, 2— low decomposition temperature of the carbonyl, 3— possibilities of controlling the hardness of the plate by adjusting the carbon content using the plating temperature and pressure as the primary variables, 4—use of high vacuum, thereby avoiding unnecessary oxidation and other complex reactions with the atmosphere. Free energy data1 show the strong tendency for titanium to combine with O2 N2 or carbon from normal temperatures to temperatures above its melting point. To maintain the titanium in a film free condition, the use of as high a vacuum as possible is indicated. The literature&apos; indicates that the reaction product of hydrogen with titanium is unstable in vacuum at around 400°C. 5—Although it is indicated from the thermodynamic standpoint that there is little possibility of removing carbon from either titanium or molybdenum, the work of Lander and Germer -ndicates that the use of a suitable H,/CO ratio is somewhat effective in minimizing carbon deposition. 6—Availability of molybdenum carbonyl. In the simplest form, the conditions of equilibrium3 in chemical reactions involving decomposition of carbonyl are as follows: Mo (CO) ? Mo + 6CO 2CO * C + CO,. The plating rate is proportional to the rate of evolution of CO from the decomposed carbonyl, i.e., it is proportional to the pressure of the gaseous decomposition products. Carbon released from CO gas is the significant constituent for the variability of the physical properties of the product. High carbon deposition is favored by increasing pressure. Limitations are imposed in the selection of plating temperature and pressure. Excessive temperature re-

Jan 1, 1956

By Lorne Roberts

"This paper describes: how Falconbridge&apos;s fire protection system meets the needs of the Lockerby Mine; why the system was chosen over other alternatives; how it is unique, but can be applied to any underground situation; details of the system; how it was installed; the role of a fire protection company; and general considerations when choosing afire-suppresant system.IntroductionIn May 1981, after about three years of searching for the best fire protection system for the re-opened Lockerby nickel mine at Whitefish, near Sudbury, Ontario, Falconbridge Nickel Mines Ltd. installed an AFFF type of fire suppression system. It was designed and supplied by the Fire Protection Systems Division of Levitt -Safety Ltd.The system protects against loss of life, equipment and/or production, and it complies with legislation should fire occur in a fuel storage area and/or scooptram garage and service bay at any or all of the three levels near Shaft No.2.About 18 months after Levitt-Safety began working with Falconbridge, the system was designed and installed at a cost considerably less than that which would be incurred if fire damage caused the loss of two days of production.The fire protection system, which overcomes a limited water supply, is a self-contained balanced pressure proportioning system. It senses the flow and automatically determines the correct concentration of foam to water. It is triggered by a release mechanism which operates a bank of nitrogen cylinders, which in turn pressurize a pressure vessel to expel the foam concentrate and water from the tanks. This solution is piped to sprinkler heads in the specific area."

Jan 1, 1982

By F. Keller, J. D. Edwards

The anodic treatment of aluminum presents problems of scientific as well as of commercial interest.l-3 Of particular interest is the fact that, during the anodic oxidation process, the oxide continues to form at the metal-oxide interface under any oxide previously formed. This has led to speculation as to the mechanism involved in the formation of the relatively thick oxide coatings that are used commercially for decorative or protective purposes. Furthermore, the ability of certain types of oxide coatings to adsorb dyes and other substances has stimulated research to determine the actual structure of these adsorptive coatings. It has been found that anodic oxide coatings on aluminum are composed essentially of aluminum oxide. They are formed by the action of oxygen ions penetrating to the metal surface during the electrolytic oxidation treatment. These coatings can be formed in a number of different electrolytes, as for example, those which contain sulphuric acid, chromic acid, oxalic acid, or boric acid. These are the commonest and most useful electrolytes employed commercially. Except for certain specific conditions of formation, the coatings in general have been found to be amorphous alumina, as far as can be determined by X-ray or electron-diffraction methods. Anodic oxidation processes can be arranged in three rather general classes if they are grouped in relation to the solvent action of the electrolyte on the coating.4 In the first class, the electrolyte has little or no solvent action on the coating that is formed. In general, coatings produced under such circumstances are nonporous and non-adsorptive. In the second class, the electrolyte exerts an appreciable solvent action on the coating. These coatings are porous and adsorptive. Finally, for the third class, the electrolyte tends to dissolve the coating about as rapidly as it is formed. This action produces electrolytic brightening or anodic polishing of the aluminum surface and at most leaves only a very thin film of oxide. The nonporous and nonadsorptive type of oxide film is represented by the coatings that are formed when solutions of boric acid are employed as the electrolyte. It is especially significant that these impervious films are formed in electrolytes that exert little or no solvent action on the coating. Where a boric acid electrolyte is used, the coating tends to form rapidly, with the result that the flow of current is soon reduced to substantially zero. This indicates that the growth of the coating has stopped. As a rule, the thickness of the coating is roughly proportional to the voltage employed for formation and the coatings of this type are exceedingly thin. In an electrolyte of this type, the coating has a high resistance when the aluminum is made anode; consequently, any current that may flow (leakage current) is very

Jan 1, 1944

By F. Keller, J. D. Edwards

The anodic treatment of aluminum presents problems of scientific as well as of commercial interest.l-3 Of particular interest is the fact that, during the anodic oxidation process, the oxide continues to form at the metal-oxide interface under any oxide previously formed. This has led to speculation as to the mechanism involved in the formation of the relatively thick oxide coatings that are used commercially for decorative or protective purposes. Furthermore, the ability of certain types of oxide coatings to adsorb dyes and other substances has stimulated research to determine the actual structure of these adsorptive coatings. It has been found that anodic oxide coatings on aluminum are composed essentially of aluminum oxide. They are formed by the action of oxygen ions penetrating to the metal surface during the electrolytic oxidation treatment. These coatings can be formed in a number of different electrolytes, as for example, those which contain sulphuric acid, chromic acid, oxalic acid, or boric acid. These are the commonest and most useful electrolytes employed commercially. Except for certain specific conditions of formation, the coatings in general have been found to be amorphous alumina, as far as can be determined by X-ray or electron-diffraction methods. Anodic oxidation processes can be arranged in three rather general classes if they are grouped in relation to the solvent action of the electrolyte on the coating.4 In the first class, the electrolyte has little or no solvent action on the coating that is formed. In general, coatings produced under such circumstances are nonporous and non-adsorptive. In the second class, the electrolyte exerts an appreciable solvent action on the coating. These coatings are porous and adsorptive. Finally, for the third class, the electrolyte tends to dissolve the coating about as rapidly as it is formed. This action produces electrolytic brightening or anodic polishing of the aluminum surface and at most leaves only a very thin film of oxide. The nonporous and nonadsorptive type of oxide film is represented by the coatings that are formed when solutions of boric acid are employed as the electrolyte. It is especially significant that these impervious films are formed in electrolytes that exert little or no solvent action on the coating. Where a boric acid electrolyte is used, the coating tends to form rapidly, with the result that the flow of current is soon reduced to substantially zero. This indicates that the growth of the coating has stopped. As a rule, the thickness of the coating is roughly proportional to the voltage employed for formation and the coatings of this type are exceedingly thin. In an electrolyte of this type, the coating has a high resistance when the aluminum is made anode; consequently, any current that may flow (leakage current) is very

Jan 1, 1944

By C. H. Li, R. D. Carnahan, R. J. Stokes, T. L. Johnston

When silver chloride deforms by pencil glide at temperatures of 26ºand 72°C, grain size has no effect upon the proportional limit and the material necks down to a knife edge under tension. At -196ºC, deformation takes place on fewer slip systems to produce straight slip traces, the flow stress becomes sensitive to grain size and fracture occurs by cleavage from an intergranular source without any reduction in area. THERE are significant differences between the appearance of the slip bands formed in silver chloride and in the alkali halides at room temperature. The bands in sodium chloride, e.g., are fine and geometrically straight, whereas in silver chloride they are coarse and wavy.&apos; Such differences in the slip behavior prompted us to inquire what the effects of grain boundaries might be on the mechanical properties of these solids. As an introduction to a general study of ionic poly-crystal behavior, we have investigated the effect of grain size on the stress-strain relationships in silver chloride at different temperatures. We have chosen silver chloride chiefly because polycrystals can be easily prepared free from cracks and macroscopic voids by conventional techniques. Moreover, as we shall see, the slip behavior can be readily modified by changing the temperature. It will be shown that the effect of grain size on the yield stress of silver chloride is strikingly dependent upon the temperature of deformation and that this temperature effect comes about through a change in the number of slip systems which operate at the onset of plastic flow. EXPERIMENTAL PROCEDURES Polycrystalline tensile specimens were made by recrystallizing cold-rolled AgCl sheet. Thirty-gram quantities of AR grade silver chloride powder were melted in a low heat capacity furnace, cast into cylindrical forms 3/4 in. in dim and approximately 1 in. in length and then extruded with a 16:l reduction ratio into rods 3/16 in. in dim. Extrusion temperatures were varied from room temperature to 350°C. In order to impart various degrees of cold&apos;work to the extruded rod. All extrusions were then cross rolled to sheet 0.040 in. in thickness at room temperature and machined to form tensile specimens having a gage length of 0.750 in. with a width of either 0.250 or 0.145 in.* Annealing was carried out in an air oven at 200°C for periods up to 20 hr. specimens having average grain diameters ranging from 0.024 to 0.40 mm were prepared by varying the extrusion temperature and annealing time in the conventional manner. To obtain specimens with grain sizes larger than 0.40mm, lightly deformed thin prisims of silver chloride single crystals (supplied by Harshaw Chemical Co.) were recrystallized. Grain size determinations were made by an intercept method and revealed that the grains were equi-axed. Laue back-reflection X-ray patterns showed little tendency to form a preferred orientation texture. Specimens which were to be used for the slip band studies were polished by immersion in fresh boiling concentrated NH,OH for 60 sec. They were then etch polished for 10 sec on each side by hand lapping on a stationary velveteen lap wetted with a dilute Hypo solution (5 g of Kodak Acid Fixer in 100 cc H20). Finally the specimens were rinsed in warm water and alcohol, blown dry and carefully mounted in the tensile machine for testing. Tensile tests were performed at three temperatures, namely, 26º, -72º, and -196°C. A screw-driven hard tensile machine was used at a constant strain rate of 0.006 in. per in. per min. Loads were determined with a light- proof ring fitted with A-18 strain gages and extensions were measured with a 0.0001 in. dial gage. Constant level baths of alcohol with dry ice and liquid nitrogen were used to maintain the two lower test temperatures. EXPERIMENTAL RESULTS Reproducibility—In view of the light sensitivity and reactive nature of silver chloride, it was necessary to determine whether reproducibility depended upon either exposure to light or to the condition of the surface. However, during the course of the work it became clear that variation of laboratory lighting

Jan 1, 1962