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By Charles M. Packer, Oleg D. Sherby, Roy H. Johnson

Originally round tensile specimens of a eutectic Zn-A1 alloy develop elliptical cross sections during superplastic deformation. This observation, coupled with a detailed study of the microstructure and preferred orieniation, suggests that crystallographic slip and continuous grain boundary migration or re-crystallization are important processes during super-plastic deformation. In spite of the extensive activity in superplasticity1-15 and the numerous explanations proposed, no single model has had universal acceptance. It has been established, however, that the general requirements for superplastic extension of two-phase alloys include an extremely fine, stabilized grain size of the order of a few microns, a temperature about equal to or greater than one-half the melting point, a critical range of strain rate, and a similarity in the mechanical strength of the major phases. The proposed models can perhaps best be characterized in terms of the important phenomena associated with them. These phenomena include: phase instability,1 diffusional creep by volume diffusion3 or grain boundary diffusion4,5 slip and continuous grain boundary migration or recrystalliza-tion,= grain boundary Sliding,7-9,13,14 and dislocation glide.'5 In this paper, experimental observations will be reported which support a model involving slip and continuous grain boundary migration or recrystalliza-tion. Specifically, a correlation will be made between this model and the development of elliptical cross sections as originally round specimens are superplas-tically deformed. For the most part, superplasticity studies have been conducted with eutectic or eutectoid alloys. Probably the most thoroughly studied material has been the monotectoid Zn-A1 alloy.1,2,6,12,13,15 No attention to the eutectic Zn-A1 alloy has previously been reported, and the results discussed in this paper represent part of a general study of the superplastic properties of this alloy. MATERIALS The alloys used in this investigation were prepared by melting appropriate quantities of 99.99+ pct A1 and 99.999 pct Zn in air, mixing, and pouring into a water- cooled stainless-steel mold. Wet-chemical analysis was conducted with each heat of alloy prepared, using the procedure of Fish and smith.16 The composition of the eutectic alloy was 95.1 wt pct Zn. Ingots about 2 in. thick were rolled to 0.4-in. plate at about 300°C with a reduction of 5 to 10 pct per pass. Specimens were machined from the plate with the tensile axis parallel to the rolling direction. The specimens were round, with 0.150-in.-diam, 1.25-in.-long gage length, and 0.25-in.-diam threaded grip sections. EXPERIMENTAL PROCEDURE Specimens were mounted inside a uniform-temperature quartz tube which was surrounded by a double elliptical radiant furnace with a 12-in.-long uniform-temperature hot zone and a low thermal capacity. The tube extended through the top and bottom of the furnace and permitted rapid quenching of the loaded specimens when quickly filled with cold water at the conclusion of the test. The quench precluded any effects on specimen microstructure from a normal, slow cool. Constant stress was applied to test specimens by suspending a load on a constant stress cam of the type described by Hopkin.17 The design of this cam permitted application of a constant stress for elongations up to 200 pct. For greater elongation, approximately constant stress conditions were maintained by systematically reducing the load manually. RESULTS As part of an investigation of the superplastic properties of the eutectic Zn-A1 alloy, evidence was obtained for the development of elliptically shaped cross sections as originally round specimens were extended. For example, after an elongation of about 100 pct, a round specimen with an initial diameter of 0.150 in. became elliptical with major and minor axis of 0.128 and 0.88 in., respectively. Photographs are presented to illustrate the ellipticity developed during superplastic deformation, Fig. 1. The specimen shown was deformed at a stress of 500 psi, at a temperature of 285°C, and a strain rate of 2.28 x 10-2 min-1. The strain-rate sensitivity exponent* was measured at *The strain-rate sensitivity exponent, m, is defined as d In o/d In c where o is the steady-state flow stress and E is the strain rate. this temperature and in the strain rate range 10"3 to 10-1 min-1 was found to be about 0.5. This value is typical of those observed with superplastic materials. The material studied exhibited negligible strain hardening during superplastic deformation, the creep rate remaining constant under constant stress and temper-

Jan 1, 1969

By J. E. Powell, F. H. Spedding

WHILE rare earths are reported to be widely distributed in nature and are not really rare," in practice, there are only a few minerals which are sufficiently rich in rare earths to serve as practical sources. Perhaps the best known of these is monazite which is a phosphate mineral containing rare earths and thorium. This mineral occurs as a dense brown sand in gravel beds and is particularly rich in the light rare earths of the cerium subgroup. This mineral is processed commercially for its thorium, cerium, and lanthanum content, and, consequently, furnishes rich concentrates from which neodymium, praseodymium, samarium, europium, and gadolinium may be obtained. Unfortunately, monazite is rather lean in rare earths heavier than gadolinium. A second mineral which is rich in the light rare earths is bastnasite, a fluoro-carbonate. Extensive deposits of this ore have been discovered in the western United States and have received considerable newspaper publicity in recent years. While bastnasite is very rich with respect to cerium, lanthanum, and neodymium, it contains even less heavy rare earths than does monazite. One of the better sources of heavy rare earths of the yttrium subgroup is gadolinite, a black silicate rock from which the rare-earth content can be extracted readily by acid leaching. It is obtained chiefly from Norway at the present time, although there are known deposits in the United States. Other sources of heavy rare earths include fergu-sonite, euxenite, and samarskite which are refractory tantalo-columbate ores. These minerals require caustic fusion or reduction to carbides with carbon before the rare-earth content can be extracted. All of the minerals which are rich in the heavy rare earths contain yttrium as a major constituent. After the rare earths have been extracted as a group from an ore by chemical means, it is generally convenient to precipitate them from acid media with oxalic acid in order to eliminate certain non-rare-earth impurities such as iron, beryllium, etc., which are usually present. The oxalate can then be readily ignited to R2O3. The oxide can be dissolved in acid and is the starting point for subsequent separation into the pure components. Perhaps the principal reason why the rare earths have not been studied as extensively as other elements of the periodic table, whose natural abundances are comparable, is that they are extremely difficult to separate from each other by the usual chemical means. Prior to 1945, the separation of one trivalent rare earth from another was a laborious process. All separations were based on repeated fractionation processes, i.e., fractional precipitation, fractional decomposition, fractional crystallization, etc. These processes were repeated from a few hundred to many thousands of times in order to obtain individual rare-earth salts of reasonable purity. Of course, mention should be made that, in the few cases where a rare earth could be oxidized or reduced to a valence state other than three, more conventional chemical means could be utilized to separate the oxidized or reduced ion from the other normally trivalent rare earths. The ionic states which deserve special mention are CeIV, SmII, Eu11, and Yb11. When it is possible to remove an element of the series efficiently, due to an optional valence state, its immediate neighbors also become easier to isolate. For example, binary mixtures of lanthanum and cerium, and praseodymium and cerium can be obtained by a relatively small number of fractional operations. The tetravalent state of cerium then allows the complete resolution of the binary mixtures by ordinary chemical means. Although the tetravalent state of cerium has been known for a long time, the divalent states of samarium, europium, and ytterbium were not used extensively in separations prior to 1930 because they are relatively unstable in aqueous media.'-" No attempt will be made to give a comprehensive review of the extensive literature dealing with the separation of rare earths. Rather, this paper will be confined to a review of those methods which have been developed at Iowa State College during recent years, and which have proved extraordinarily successful for the isolation of highly pure rare earths in quantity. It was obvious that, if pure rare earths were to become generally available, methods would have to be developed wherein the thousands of fractional operations made necessary by the similarity of rare-earth properties could be performed automatically. The development of chromatographic techniques and ion-exchange resins appeared to offer a mechanism by which this objective could be accomplished. A number of early attempts were made to separate rare earths by these means; for example, Russell and Pearce12 passed a mixture of rare earths through a cation-exchange column and reported

Jan 1, 1955

By A. M. Skov, L. F. Elkins

First response to large-scale water flooding in the fractured very low permeability Spraberry sand has led to a new unique cyclic operation. Capacity water injection is used to restore reservoir pressure. This is followed by marly months production without water irzjection and the cycle repeated. Expansion of the oil, rock and water during pressure decline expels part of the fluids but capillary forces hold much of the injected water in the rock. At least with reservoir pressure restored and with partial water flood development, field performance has proved this cyclic operation is capable of producing oil from the nzatrix rock at least 50 per cent faster and with lower water percentage than is imbibition of water at stable reservoir pressure. INTRODUCTION The Spraberry Field of West Texas presents unusual problems for both primary production and water flooding. Extensive interconnected vertical fractures in the fractional-md sandstone permitted recovery of oil on 160-acre well spacing, but they made capillary end effects dominant. Primary recovery by solution gas drive is less than 10 per cent of oil in place. The concept of displacement of oil from the sand matrix by capillary irnbibition of water has led to field techniques which promise greatly increased oil recovery. Free exchange of laboratory research, reservoir information and results of field pilot tests among the various companies has been very important in development of this technology. Five units covering a total of 170,000 acres have been formed for water flooding, and 10 other areas covering an additional 175,500 acres are in various stages of unitization. Part of the Driver Unit reaching fillup first has demonstrated very unusual waterflood behavior and indicated numerous operating problems that will develop within and among the various units. SPRABERRY ROCK AND PRIMARY PERFORMANCE The Spraberry, discovered in February, 1949, is a 1,000-ft section of sandstones, shales and limestones with two main oil productive members: a 10-15 ft sand near the top and a 10-15 ft sand near the base. In part of the field some thinner intermediate sands are oil productive, and others are water bearing. All sands have permeabilities of 1 md or less and porosities of 8-15 per cent. Ordinary core analysis and electric and radiation logs are ineffective in differentiating between oil productive and nonprcductive sands. Sands capable of containing producible oil are best identified by mercury injection capillary pressure measurement and, in some cases, by core water saturation. About 3,500 wells have been drilled in the 500,000-acre trend. Vertical fractures were observed in practically all Spraberry cores. Continuity and interconnection of fractures were confirmed by pressure interference among wells during early development.' Major fractures trend northeast-southwest as indicated by oriented cores and confirmed by five fluid injection tests, by analysis of the pressure transients observed during development,''' and by three interference tests in the Driver Unit Water Flood reported herein. Fracture spac- ing probably averages inches to a few feet. Spraberry wells typically produced 100-400 BOPD initially after hydrauLic fracture treatments. By 1962 oil production had declined to an average of 12 bbl/well/day, near the economic Limits of operation. Reservoir pressure had declined from 2,300 psi initially in the Upper Spraberry and 2,500 psi in the Lower Spraberry to 500-1,000 psi. Partial closing of the fractures with declining reservoir pressure is believed to be the cause of such low oil production rates at these relatively high reservoir pressures. Cumulative recovery of 208 million bbl of oil is 80 to 90 per cent of that recoverable by primary means. Performance of the entire reservoir is summarized in Fig. 1. IMBIBITION WATER FLOODING By 1952 reservoir performance indicated low primary recoveries. Most engineers, expecting serious channeling of injected fluids through the fractures, held little hope for secondary recovery. With its extensive background of research on the fundamentals of fluid flow within reservoir rocks, Atlantic's Research and Development Division on short notice in 1952 conceived that displacement of oil by capillary imbibition of water into the rock might significantly increase Spraberry recovery. Laboratory data reported by Brownscombe and Dyes scaled to probable reservoir conditions showed potential waterflood recovery equal to or greater than primary recovery with a 10-15 year flood life.= A pilot test using three 40-acre injection wells, one central producing well and 18 surrounding observation wells demonstrated technical feasibility of the process. Injection of 1.5 million bbl of water from November 1952 to August 1955 proved water entered the rock and displaced oil

By P. Hanniala, S. Harkki, B. Andersson

"The Outokumpu Flash Smelting Process was put into commercial operation in 1949. The original process was based on the use of preheated air. The adoption of oxygen enrichment of the flash smelting process air in 1971 was a crucial improvement, especially for smelter capacity. Oxygen use according to the Outokumpu method means selection of the most suitable oxygen content for the process air on the basis of the concentrate composition, capacity and matte grade. The furnace is not bound to only one fixed degree of process air oxygen enrichment; the oxygen content may vary from 21% to 100%.The degree of oxygen enrichment and the matte grade are the most important process parameters in reducing the operating costs of the whole system, including smelting, converting and acid production. Raising the matte grade allows more efficient use of the reaction heat in the smelting stage. Sulphur is recovered in a high-strength, constant-flow gas stream. The blowing time in the converters is reduced considerably.Oxygen enrichment and high matte grade improve the energy efficiency of the plant complex as long as the surplus heat from the system is not wasted. When the operating costs and investment expenditure of the total plant complex are taken into account, a reasonably high degree of oxygen enrichment (35-80°/0) is the best alternative in practice. Existing operating smelters have achieved single-stream thoughputs of over one million t/yr of concentrates.HistoryLocal capital and operating costs as well as lower energy consumption per unit of metal produced are now the crucial factors in determining the choice of process. In the late I940s, the same reasons prompted Outokumpu to develop the original flash smelting process in Finland. Between 1900 and 1940, very few technical changes in pyrometallurgical copper production took place. However, the commercial use of the flash smelting technique began a new era in metal extraction from sulphide concentrates. The characteristic feature of the method is that the concentrate is smelted in suspension: this offers the most favourable conditions for heat and mass transfer, and thus high reaction velocities. Outokumpu was the first to exploit the known advantages of flash smelting in a commercial installation at Harjavalta in 1949."

Jan 1, 1982

By Clarence G. Merritt

Stainless iron, as mild stainless steel is usually called, an alloy ranging from 11.50 to 15.00 per cent chromium with carbon under 0.12 per cent, has been considered to be not appreciably affected in respect to corrosion resistance by heat treatment. This metal, while one of the most widely used of the "straight" chromium stainless alloys, has failed in many applications because of insufficient information regarding heat treatment. These failures have been attributed to many possible causes from an inherent lack of resistance to corrosion and misapplication to mlysterious electrolytic effects or comparatively minute non metallic inclusions. Many uses for a steel with such excellent physical properties as are latent in this alloy have been lost on account of corrosion failures which could have been avoided by applying proper heat treatment. The alloy has not received the recognition or attention it should because of the fact that the details of its metallurgical behavior were not thoroughly understood. Response to heat treatment of the steel is well known as regards tensile properties,1-2 but its application has been for improvement in tensile characteristics or on account of machining considerations rather than for corrosion prevention. The potential user of this steel has not been clearly advised in papers, either technical or commercial, that have been written about it in the last 10 years or more, of particular features that are of prime importance in developing the excellent properties of this metal. The data to be presented in this paper are concerned mainly with the effect of heat treatment on the corrosion resistance, but a study has also been made of the concurrent microstructural changes and an explanation developed for the phenomena revealed, as well as a correlation to the other physical properties—hardness, tensile characteristics and impact strength. Stainless steel, largely used for cutlery purposes, an alloy of approximately 13.00 per cent Cr with 0.30 per cent C;, must be hardened and the surface prepared by polishing or pickling for best resistance to staining and corrosion. Monypenny reports that a loss of hardness is

Jan 1, 1932

By D. A. Whitley, R. P. Carone

"Shaft sinking by blind shaft drilling offers the mining industry a different approach to shaft construction. Benefits of blind drilling include less construction time and fewer safety problems while being economically competitive with conventional sinking methods under certain conditions in soft water-bearing formations.Technology and equipment are available today to drill blind shafts up to 20 feet in diameter and over 3,000 feet deep. This is an extension of proven techniques developed by private industry. To drill a 20-foot-diameter hole requires a specially manufactured hydraulic drill unit with a rated hoist of 2 million pounds and 500,000 ft/lb of torque.This brief paper will discuss the following aspects of blind shaft drilling:• benefits;• equipment f or drilling;• circulation methods;• circulation rates;• shaft alignment; and• progress rates to be expected.IntroductionShaft sinking by blind shaft drilling offers the mining industry an improved alternative method for shaft construction. The drilling of 20-foot -diameter shafts to depth s in excess of 3,000 feet can be done by utilizing equipment specifically designed and manufactured for this purpose. This equipment is a distant cousin, at best, to standard oil well drilling rigs. The actual configuration of these drilling machines will be discussed in a following section.To most people, the drilling of mine shafts may seem to be a new or at least recent technology. However, as early as the I920s, German and Dutch miners were drilling 24-foot diameter shafts for coal mines. What led ""miners to resort to drilling were ground conditions that still plague conventional shaft sinkers today: soft , water-bearing formations. The major drawback to these early attempts was a low penetration rate due to poor bit cleaning. This, however, was not the end of early shaft drilling activity. From 1936 to 1950, a number of mine shafts were drilled by the calyx or coring method. This method employs a bit with a large bore down the center. As it drills, it cuts a core. When 5 to 10 feet have been drilled, the core is removed. The disadvantages of this method were the time and work involved in breaking the core free, and it was inadequate in soft water-bearing ground."

Jan 1, 1981

By Wilson T. Lundy

The history of the production of sulfur from salt domes in Louisiana and Texas originated with the operations of the Union Sulphur CO. at Sulphur, La., followed by the Freeport Sulphur Co. at Bryanmound, Tex. Including the present development of Grande Ecaille by the Free-port Sulphur Co., which constitutes the tenth dome to be equipped for the production of sulfur in the Gulf Coast, less than 10 per cent of all the known domes have proved to contain sulfur in commercial quantities. The Grande Ecaille salt dome is in the tidal marsh of the Mississippi River delta in Plaquemines Parish, Louisiana. It is 10 miles southwest of the right descending bank of the river approximately 45 miles below the city of New Orleans and is within 4 miles of the shore line of the Gulf of Mexico. Terrain Characteristic of the delta region, the terrain consists of a low, flat, uninhabited area of marsh land intersected by many shallow lakes and bayous. With the exception of salt grasses, the region is devoid of vegetation and presents, in all directions, an unobstructed path to the vagaries of the winds. The general character of this area can be best visualized from the mechanism of its formation.' Offshore bars formed enclosing long narrow lagoons between the bar and the inner shore line, the lagoons communicating with the sea by means of tidal inlets. The water in the lagoons, being comparatively quiet, favored the deposition of fine debris composed of sand carried into the lagoons by action of the waves, tides and river-borne sediments from the land surface. As this material accumulated the bottoms of the lagoons were built up and eventually salt grasses obtained a foothold. The successions of growth and decay of these grasses formed a brown fibrous mat varying in depth from a few inches to several feet. This mat of vegetation virtually floats on an ooze that is several feet thick and is composed of alluvial sediments and very fine sand, and the whole is underlain by an unctuous clay. The decayed vegetation from the upper layer when dried has a peaty appearance.

Jan 1, 1934

By Cyril Wells, Robert F. Mehl

The purpose of this investigation was to prepare high-purity iron-carbon alloys, to determine as precisely as possible the A3(GOS), the Acm(SE), and the A1(PSK) transformation temperatures in the meta-stable iron-iron carbide system (up to 1.4 per cent C), and to study the influence of carefully controlled and constant rates of heating and cooling (1/8 to 2o C. per minute) upon the transformation temperature and upon the resulting microstructure. Apart from the general metallurgical importance attending the completion of such a task, it will be noted that highly precise transformation temperatures are of interest and importance in the thermodynamic study of this system1. Several determinations of the iron-iron carbide diagram have been made2. These suffer generally from the low purity of the alloys used, and from the application of methods of investigation of low sensitivity. Attempts to compare and weight the many data available in an effort to construct as accurate a diagram as possible have, in the main, been unsuccessful. In general, the wide differences in the results of different workers, the lack of complete analytical data, the omission of important details relating to the heat-treatment of the alloys, and the meager description of the methods of investigation applied, render such a process of averaging nearly meaningless. It may be seen from the summaries by Epstein2 and Körber and Oelsenl that variations as great as 30' C. exist in the reported data on the A3 temperatures in iron-carbon alloys. Fortunately, the Aa temperature in pure iron is now known to be 910" C. ± 1° C.3 The best recent work on iron-carbon alloys is that of Esser4 on hypoeutectoid steels and that of Sato5 on both hypoeutectoid and hyper-eutectoid steels. Esser made a dilatometric and magnetic study of iron and iron-carbon alloys containing 0.06 to 0.86 per cent C, for which a high purity is claimed. Presumably the electrolytic iron was reasonably pure, but the alloys contained considerable impurities, on the average totaling 0.35 per

Jan 1, 1937

By James K. Stanley

When a plastically deformed mctal is heated to a certain temperature, it undergoes a complete change in microstructure, the consequence of which is a marked alteration of mechanical properties such as hardness, strength and ductility. This change in microstructure occurs by re-crystallization and is a process involving the formation and growth of strain-free nuclei in the deformed matrix. These nuclei continue to form with time and grow until a new grain structure replaces the cold-worked structure. The formation of the nuclei in the deformed sheet of I per cent silicon ferrite is illustrated in Fig. I. If a recrystallization is conducted iso-thermally, a nleasurement of the fraction of the matrix recrystallized plotted against time leads to an isothermal recrystallization curve, first established in 1942.1 Such recrystallization curves are shown in Fig. 4. These curves show that the recrystallization of a cold-worked metal is best considered as a rate process rather than a time independent process such as is suggcsted by the improperly named and misleading recrystallization diagrams involving deformation, temperature, and grain size.2-5 Any study of the rate of recrystallization resolves itself into a study of the component rates of nucleation and growth. The previous paper1 provided an account of the determination of the rates of nucleation; N, the number of nuclei formed per unit time per unit of unre-crystallized area, and growth, G, the radial growth in unit time, in the recrystallization of silicon ferrite (I per cent Si). A method was developed to furnish experimental data for evaluating the effect of the recrystallization variables on N and G. The mathematical analysis for the derivation of the isothermal recrystallization curve was developed for a two-dimensional case (in thin sheets where the diameter of the recrystallized grain is greater than the sheet thickness). The present paper is a continuation of the study of recrystallization of I per cent silicon ferrite begun in 1942.1 In this work the effect of the factors deformation, temperature, grain size, composition, and recovery is studied with respect to the rates of liucleation and grouth. At the same time it is shown how the cooperation of N and G affects the isothermal recrystallization curve. The study of these variables on N and G has a definite bearing on the mechanism of recrystallization and should lay a foundation for a rational theory on the subject. Procedure The procedure used in these experiments was essentially the same as that described previously but in certain details some changes were made in the interests of speed. With few exceptions, the procedure is the same for the study of all the variables. Where the procedure is different from standard manipulations attention is called to this fact.

Jan 1, 1945

By George J. Clark

One of the major problems of operation in the anthracite industry is the disposal and handling of refuse—not because of its complexity but because of the quantity and type of material involved. It is the purpose of this paper to describe the kinds of refuse, methods of disposal, quantities of material to be handled and equipment used, together with present day application at specific operations in the Northern, Eastern Middle, Western Middle and Southern anthracite fields. For the purpose of this paper, refuse is considered to be any material that has no present or foreseeable future value and that must be handled and disposed of in the process of mining and preparing anthracite for market. Included in this classification are tunnel rock, mine rock, cleaner plant refuse, breaker refuse, old timber, ashes and silt. Disposal Methods Old timber is disposed of either by burning or by depositing on the refuse bank. Burning is preferred because timber on the refuse bank is a potential fire hazard. Ashes are deposited on a separate bank, mixed with other refuse, or flushed into old mine workings. In many places, the latter practice has caused considerable difficulty in preparation of coal mined from these areas. In depositing ashes on the surface, it is wise to refrain from mixing them with material containing coal as such contamination may prevent reclamation of the coal in future years. Tunnel work, mine rock, cleaner plant and breaker refuse compose the bulk of the material to be disposed of and handled, and are referred to collectively as "refuse" in this paper. Waste material in or adjacent to the coal beds may be removed at the working face wherever possible. This can be done in flat or lightly pitching beds, and in the Northern field represents a sizable percentage of this type of refuse handled. In the other three coal fields, this method of disposal cannot often be used. Refuse not removed at the working face is taken to the surface and generally is deposited on banks; occasionally it is crushed and flushed into old mine workings. Breaker refuse often is used for constructing berms for silt-retention basins. Disposal Problems The problem of handling refuse is different for each operation, owing to topographical conditions, quantity of material to be handled, anticipated requirements and types of equipment in use elsewhere at the operation. Preparation plants with limited refuse-disposal areas, excessive grades to reach the required elevation and long hauls to disposal areas not readily accessible require the selection of equipment to best meet the conditions. The quantity of refuse to be handled from a given amount of raw material varies considerably throughout the four fields. In mine coal, this varies from a low

Jan 1, 1949

By R. C. J. Goode, W. S. Rapson, W. R. Lawrie, L. W. P. Van Der Bosch

W. R. Lawrie (Member): As all the Institute members present are aware, the Ninth Commonwealth Mining and Metallurgical Congress was held in Great Britain from 3rd to 24th May, 1969. The Congress opened in London and the first week was devoted to technical sessions. Several receptions and other forms of entertainment were held in the evenings. The Congress was attended by some 1 200 delegates, many of whom were accompanied by their wives. As can be imagined a large organisation was needed to cater for all the whims of these delegates, to arrange accommodation and to provide transport for the technical trips, for the receptions and for the sight-seeing tours. Papers presented at the technical sessions proved of great interest. It was stimulating to hear of the developments taking place in the various branches of mining and metallurgy. The discussions which developed between men from so many different countries were thought provoking, led to new friendships and most of us made valuable contacts for the future. There were 141 papers presented in the one week. They were given in four separate halls with two, three and sometimes four papers coming up for discussion in each of the three sessions per day in each hall. Among the more interesting subjects were those concerning off-shore drilling and the facilities for production of petroleum and natural gas. Beach mining at Consolidated Diamond Mines drew a large audience. Automation, mechanization and other technical developments were well described and we were brought up to date with modern techniques of mineral prospecting. There was general discussion on the future of the mineral industries together with comments on the consumption and price trends of these metals and minerals. The future of uranium, of vital interest to us in South Africa, came in for much debate. During the first week, besides attending the technical sessions and seeing some of the sights of London, we were royally entertained. There was a banquet, attended by some I 400 people, where we were welcomed by Princess Alexandra, a reception by H.M. Government in the Banqueting House, and we were entertained at the House of Lords on a terrace overlooking the bustling and rather muddy river Thames. Then there was the visit to the Glyndebourne Opera. It is only in London that at 3 o'clock of an afternoon, nearly 1 000 people all togged up in dress suits and long dresses and carrying packets of sandwiches for supper could arrive at a station to catch a train, and not even cause a stir of interest or a raised eyebrow! This is the way we travelled 60 miles to the opera from London. Surely there can be no more picturesque or romantic a setting for an opera than this large 400-year old red brick manor house nestling in the green valleys of the unspoilt Sussex countryside. It was a glorious evening and though we returned somewhat late and tired, not one of us would have missed this experience. After the first week in London there was a choice of tours of one week to London and the Home Counties, Cornwall, a Geological tour to Scotland, South Wales, and North England. These were followed by further one week tours to Yorkshire and Lancashire, Scotland, West Country and Midlands, a Geological tour of Wales, and a Mining and Geological tour to Jurassic Iron Mines. We then returned to London for the final session and closing banquet. Post-congress tours were arranged to Europe and to Ireland. It was a wonderful Congress, a great experience, we made many friends and may there be many more congresses! . L. W. P. van den Bosch (Member): Much has already been said in appreciation of the excellent organisation and arrangements made for the delegates who attended this Congress. This report is confined to a brief discussion of the personal impressions gained from the papers presented and the technical visits attended. The papers covered a wide variety of subjects ranging from highly theoretical observations to practical descriptions of operations. There were three main themes, VIZ: 1. The attention given to research and its forceful application to practical operation. 2. A steady development in mechanization and automation leading to savings in manpower. 3. Improvization, modernization and adaptation of exisitng facilities. Thoughts on these themes can best be illustrated by comments on some of the industries visited. COAL The National Coal Board (N.C.B.) has been most progressive and all of us have heard of the Bevercotes Colliery with its completely automatic mining and coal handling equipment. This was not, unfortunately, on show but there is no doubt that this is one of the greatest advances in coal mining leading towards continuous production. Coal in Britain is fighting for its life against oil, North Sea gas, imported gases and nuclear power. Output is dropping, the less efficient collieries are closing down and efficiencies are steadily rising as the following tabulation indicates: In 1931: 1 million men produced 300 million tons of coal In 1947: 0.7 million men produced 230 million tons of coal In 1968: 0.4 million men produced 160 million tons of coal

COUNCIL The following served on Council during the year under review: Office bearers: Messrs V. C. Robinson (President), Prof D. D. Howat and Dr J. P. Hugo (Vice-Presidents), J. K. E. Douglas (Immediate Past President) and D. G. Maxwell (Honorary Treasurer). Ordinary Members of Council: Dr M. G. Atmore, Dr J. M. Bereza, H. P. Carlisle, W. W. Malan, C. E. Mavrocordatos, Prof R. P. Plewman, Dr R. E. Robinson, Dr M. D. G. Salamon, P. W. J. van Rensburg, L. W. P. van den Bosch, P. A. von Wielligh. Branch Chairmen: J. Meintjes, J. M. Meyer (Acting), J. N. Saunders (Retired). Past Presidents serving on Council: R. J. Adamson, M. Barcza, H. Britten, R. C. J. Goode, P. Lambooy, Prof J. de V. Lambrechts, Dr J. T. Mclntyre, J. F. Reid, H. Simon. Ten Council meetings were held during the year with an average attendance of eighteen and the standing committees held forty-six meetings. FINANCE The annual accounts, which are attached to this report, show an excess of income over expenditure of R5 051 compared with an excess of expenditure over income last year of R4 608. This major reversal of fortunes is due in the first instance, of course, to the increased subscriptions. There were, however, other important contributors, particularly sales of the Proceedings of the Symposium on Open Pit Mining and profits on the operation of symposia and colloquia. It would appear from a study of the accounts that there has been a substantial drop in expenditure on secretarial fees. In actual fact, however, our total expenditure on secretarial fees was higher. A portion of this expenditure was charged against the administration of the Symposium on Open Pit Mining and, in addition, the charge against the Journal accounts for secretarial fees was increased. It will be recalled that in last year's annual report it was mentioned that subsequent to the new arrangement for publication of the Journal, the expected improvement in the finances of the Journal had been slow in materialising. After a total period of 18 months there was still no sign of improvement and it was accordingly decided to end the arrangement. As a result, the drain on the finances of the Institute was considerably lessened in the second half of the year. During the course of the year Council became concerned about the rapid depletion of our accumulated funds and gave careful and detailed attention to all aspects of the Institute's financial affairs. Particular attention was given to: 1. The fact that the Institute does not have a solid financial backing and must appeal for funds every time any special event such as a symposium is held. 2. The responsibilities of the Institute to the profession and the community, with particular reference to the desirability of establishing Institute bursaries and participating in other educational activities. 3. The rapidly rising cost of living. 4. The immediate financial position of the Institute. 5. The rapidly increasing cost of publishing the Journal due to the increasing number of papers available. In the meantime the immediate financial position of the Institute has improved but as this is due largely to non-recurring or irregular items of revenue, it should not be given undue weight. After careful consideration it was decided that an appeal should be made to industry for financial assistance, which would be used to cover the cost of symposia and other unusual expenditure and also, if possible, to build up the capital resources of the Institute so that there is a solid foundation for the future. Before appealing to industry, Council wished to be quite certain that there could be no criticism of the Institute for not having done our best in a personal capacity. Furthermore, Council examined many comparative statistics, including those circulated to members, which showed that, while expenditure per member has risen at an average annual rate of 7,5% over the last fifteen years, subscription revenue per member has risen at only 3,4% per annum. It was with this background that your Council decided to raise the subscriptions. Initial approaches have been made to the big mining groups and there has been a very generous response, although the details of how financial assistance will be provided have not yet been worked out. It seems likely that some form of affiliated company membership will be the most suitable method of achieving this. When these details have been fixed, it is the intention to extend the appeal to all corners of the mining industry as well as manufacturing and metallurgical industries. It is believed that these measures will ensure that the finances of the Institute are placed on a firm foundation on which the expanding activities can be planned. The MacArthur Forrest Memorial Fund shows an excess of income over expenditure of R73 and the total fund was, therefore, increased by this amount to R4 411. The balance sheet shows that the market value of quoted shares and debentures increased during the year fron R6 540 to R9 160. The market value is now almost exactly the same as the book value. Accumulated funds now amount to R23 010 compared with R17 959 a year ago.

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

By F. C. Pittman, D. W. Harriman, J. C. St. John

This paper mentions briefly the history of hydraulic jetting as applied to perforating and fracture initiation. It points out the advantages of hydraulic perforation and undercutting as an aid for creating a fracture at the point desired rather than depending upon the weakest point in the formation for breakdown. It describes early experimental work with jet nozzles in search of better nozzle materials. The effect of splash-back damage and its subsequent influence on jet body and tool design during this work is discussed. A series of cutting-rate curves for jets cutting steel and steel-cement-formation combinations is presented to show the effect of hydrostatic head and the point of diminishing returns with respect to cutting time. There is a series of photographs showing various types of rock formation in which perforation and undercutting tests were made. These stones were drilled and the casing cemented in place as in an actual well. The casing was perforated and circularly cut as if preparing for a fracturing job. The conclusion reached in the paper is that hydraulic jetting with sand-laden fluid can be used for perforating and undercutting casing, cement and formation rock for the intended purpose of inducing the formation to fracture at a desired point. INTRODUCTION Hydraulic jetting as a means of cleaning a formation during acidizing has been used for many years. The acid-jet gun was used to clean formation and for drilling cement from casing with acid. This tool was dropped to a seating ring installed on the tubing and could be retrieved by reverse circulation or wire line. In this process, the fluids were directed against the formation to clean and penetrate beyond the mud-damaged area. After the development of the hydraulic fracturing process, interest in jetting the formation with abrasive-laden fluid was renewed. The cutting action of abrasive fluid on pumping equipment, which is a well known problem, has been utilized to perforate and undercut casing, tubing and formation. In this process, surface areas are provided in the formation on which the frac- turing pressures may work to produce a fracture at the location desired. EQUIPMENT The tools used consist of bodies containing two, three or four jets in a single horizontal plane equally spaced around the circumference. The body is threaded to the end of a string of tubing and run into the well. In addition, an expendable tool is available that may be left in the hole after perforating and produced through until necessary to remove the tubing. The bottom of each tool is equipped with a ball-type back-pressure valve. The ball can be reversed to the surface and recovered. This allows reverse circulation so that loose sand which accumulated below the tool while jetting may be removed before the fracturing job. The present jetting tools are of such length that, when screwed together, the jets fall on 12-in. spacing. ANALYSIS OF THE PROBLEM Early work with nozzles indicated that hardened steel was not a suitable material for jets and that more durable material would be required. Ceramics were tried and found to be superior to steel but still too shortlived for most applications. Tungsten carbide, which was tried and found to be the best material available, is now being used for jet nozzles. Analysis of the problems presented by this process indicated that the following information was needed. 1. The effect of submergence on a jet stream and the effect of submergence on the cutting rate of a jet stream. 2. The cutting rate and depth of a jet stream in steel. 3. The cutting rate in various formations and point of diminishing returns. 4. Size of hole or slot cut in a pipe by a given jet. 5. Fluids and sands used. 6. The flow of various weight fluids through the jet nozzle and the discharge coefficients. 7. The type cut formed in the formation by the jet stream. 8. The stretch and contraction of tubing due to temperature and pressure. The cutting effect of a jet stream on a target in the atmosphere is rapid and spectacular as most of the

By H. W. Schadler

The superplastic behavior of low carbon and manganese bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests are reported which indicate that high strain rate sensitivity (>0.5) and adequate elongations are achievable in ultrafine-grained steels 1 to 2 p, but at strain rates which are not commercially attractive. It has been demonstrated that the fine grain size is retained after long times and high strains if the temperature is kept within the range of the two-phase (a + ?) field. INTEREST in superplasticity has been stimulated by the desire to: 1) understand the origin of, and mechanisms responsible for, the large uniform elongations observed, and 2) exploit this property for commercial advantage in metal forming operations. Although the Zn-22 wt pct Al alloy presently being studied as a model material1-5 may find application in sheet forming and extrusion, the potential of super-plasticity should best be realized in large tonnage materials, such as steel and aluminum alloys. The degree of superplasticity in low-carbon and manganese-bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests on ultrafine grain size material are reported. Avery and Backofen6 and Hart7 have shown that geometrically stable flow leading to extensive uniform elongation in the tension test is associated with high values of the strain rate sensitivity, m, defined: Lozinsky had reported that titanium and zirconium experience permanent deformation if subjected to a constant load and cyclic heating through the temperature range of the phase transformation. Although strain rate sensitivities in excess of about 0.2 had not been reported previously for steel, permanent deformation had been observed11-13 in a wide variety of steels subjected to a constant load and cyclic heating through the temperature range of the a-? phase transformation. Thus by analogy, steel could be expected to exhibit high strain rate sensitivity but only in the a + ? condition. High strain rate sensitivity has been observed at 650°C (a + Fe3C), but not reported as such, by Bailey, Dickenson, and pearson14 in 1931 at a strain rate of about 10-9 per min. It then remained to determine whether high tensile elongations would be observed in a rate-controlled test at constant temperature and at what strain rate strain rate sensitivity values greater than 0.5 would be observed. Since previous experience8 had indicated the importance of fine grain size to realizing high m at reasonable strain rates, it was first necessary to produce an ultrafine grain size and then keep the grains from growing during the test. The results of this investigation show that fine grain size can be readily produced16 and maintained by restricting the temperature of testing to below the ? transus. Further, superplasticity (high m and large uniform elongation) is observed. However, the strain rate range is only marginally useful for commercial forming operations with the finest grain size produced. MATERIAL The material investigated initially was a 1.9 wt pct Mn, 0.42 wt pct C, hot-rolled bar previously used by Low and Turka1015 and available in the laboratory. The 0.500-in. round was cold-rolled to a 0.090-in. flat, annealed for 4 hr at 850°C in argon, air-cooled, and cold-finished to 0.050 in. Subsequently, four additional steels of the compositions given in Table I were investigated to explore the effects of manganese, carbon, and test temperature on the observed stress-strain rate behavior. These steels were melted under argon, cast to 0.75 by 2 by 5 in. slabs, hot-rolled at 850°C, surface-finished to 0.13 in., and cold-finished to 0.050 in. Sheet tensile specimens 0.200 in. x thickness with 1- or 2-in. gage length were cut parallel to the rolling direction. Table I also includes the nominal transformation temperatures for the AISI 1340 and the four experimental steels. EXPERIMENTAL PROCEDURE Production of Fine Grain Size. Ultrafine grain size (1 to 5 p) was considered essential for this studv. Grange16 has described two techniques for producing

Jan 1, 1969

By Frank Doxey

AT Dominion Steel & Coal Corp. it has long been recognized that continued mechanization of mine operations is necessary in the Pictou, Cumberland, and Sidney coal fields of Nova Scotia. The varied physical conditions in these fields call for special consideration of individual cases before planning is finalized. Because standard equipment cannot be procured which would operate successfully, many experiments have been necessary over the years to keep pace with the progress made in other countries. There are two mines, producing 2000 tpd, located in the Pictou coal field. The field is badly distorted and crossed by many faults. Seams are highly inclined and irregular and vary in thickness from 5 to 40 ft. Entries are difficult to maintain because of squeezing of the coal. ribs and movement of the roof and pavement. Output from the three operating mines in the Cumberland field is 3000 tpd. The field is highly inclined, inclination varying from 12° to 32°. Overlying beds consist of shales and massive sandstone lenses of extreme toughness and are responsible for bumps when the stresses are relieved by extraction. At greatest depth these are among the deepest coal workings in the world. Depth of cover ranges from 2300 to 4000 ft. This prohibits room-and-pillar working and necessitates longwall operation. Working of contiguous seams concurrently to maintain output increases the already difficult conditions. The Sydney field, with a frontage of about 30 miles, is the most important of the Nova Scotia coal fields. With the exception of one small area it is now wholly submarine. Output is approximately 21,000 tpd. Seams are 21/2 to 8 ft thick, and cover in the areas varies from 600 to 2300 ft, with an average of 1500 ft from sea bottom to the top of the seam. The seams dip in a seaward direction, pitches ranging from 6" to 4.0". The shoreline is the last place of entry to the seams and distance from the bank to the working faces is generally over 3½ miles, in some cases as much as 6½ miles. Ventilation is a problem and requires the construction of large permanent airways. Getting and Loading Coal: In 1925, in view of heavy pressures exerted by thickness of cover overlying the seams, roadways and pillars of the room-and-pillar system being worked began to break up and coal was lost. It was decided that a change in the method of extraction in areas with heavy cover was necessary, and experiments were made with many short walls and longwalls varying between 90 and 250 ft. Trial and error proved that the best operating length was between 400 and 500 ft, delivering all coal to the dip, with roadways to the face following a level course. The change-over was gradual, and the technique of roof control developed with the system, so that falls to the face are now very infrequent. An advantage of longwall mining is that it yields 95 pct extraction, especially important in coal seams of high quality or in seams where faults or disturbances restrict the workable areas. This percentage of extraction is based on the fact that the longwall advancing system takes development faces where pitch permits instead of driving headings and leaving roadway pillars. This system yields high tonnage during development and limits loss in extraction to duff left during operations. Accompanying disadvantages, on the other hand, are the heavy construction cost of main roadways and the necessity of driving all new flank face roadways through the gob. If the main roadways are driven through the solid, and large enough pillars are left on each side for protection against flank face weights, then the width of solid coal is approximately 1700 ft. This represents 10.6 pct of the coal available, or 89.4 pct extraction of the whole. These pillars, however, are of such size that they provide a useful pillar drawing area as a final operation of the mine. It may be that although the seam cannot be generally mined by the room-and-pillar method, it can be adapted to

Jan 1, 1955

By Donald B. Evans, Robert D. Pehlke

The solubility of nilrogen in liquid binary alloys of iron with Litanium. zivconium, columbium, vanndiurn, and tantalum was measured for alloy composiLions up to the solalbility limils of lhe alloy nitrides. All five alloying agents were found to decrease markedly the activity coefficient of nitrogen in liquid ivon. The metal/nitvogen mole ralios in the alloy nitrides formed were generally .found to be slighlly greater than 1.0, but in no case greater than 1.5. From the experimental data, the standard free energies of fortmation of titanium and zir-conium nitrides have been calculated for the Lemperaluve range 1550° to 1750 C. The solublily Products for columbium, tantalum, and vanadium nitrides are also reported. A number of research investigations have examined the effect of refractory metals on the solubility of nitrogen in liquid iron. Although data on zirconium are not available, investigators are in agreement that titanium, vanadium, columbium, and tantalum markedly increase the solubility of nitrogen in liquid iron. This fact alone makes desirable the acquisition of thermodynamic data for these elements in liquid iron. Since refractory metals are known to be stable nitride formers, they have been suggested as steel denitrifying agents, and some of their nitrides have recently been considered as containment materials for liquid iron and iron alloys. Most available thermodynamic data for these metals relate to their dilute concentrations, but effective thermodynamic treatment of these applications requires data at concentrations near the solubility limit of the alloy nitride. Although some work has been done at relatively high alloy concentrations in liquid iron (particularly for vanadium 2,3 and titanium 2,4), the results have been somewhat contradictory. Disagreement may be partly attributed to the fact that the compositions of most refractory metal nitrides have been shown to be nonstoichiometric, and to vary 2,5-8 depending on the temperature and nitrogen gas pressure with which the solid nitride phase is in equilibrium. One purpose of this study consequently has been to determine the compositions of the refractory metal nitrides precipitated from a liquid iron solution. EXPERIMENTAL PROCEDURE Rao and Parlee2 and Evans and Pehlke 9 have discussed the technique for measuring the solubility product of an alloy nitride phase in liquid iron by finding the point of departure of the nitrogen solubility from Sieverts' law. The method consists of measuring the solubility of nitrogen in a melt of iron containing a known concentration of a second metal as a function of the nitrogen gas pressure over the melt. In this study the second metal was one of the refractory metals titanium, zirconium, columbium, vanadium, or tantalum. When the nitrogen pressure at which the refractory nitride forms is reached, a deviation of the measured solubility of nitrogen in the melt from Sieverts' law is observed in the form of a "pressure halt." The concentration of nitrogen in the melt associated with this breakpoint in the nitrogen-absorption curve is then used to calculate the nitride solubility. The Sieverts method was used to measure nitrogen solubility as a function of nitrogen pressure and temperature. The experimental equipment for this technique has been previously described in detail. 1,9 Charge materials used were vacuum-melted high-purity iron (Ferrovac-E) and the best commercial grades of the refractory metals obtainable (in all cases at least 99.8+ pct pure). Recrystallized alumina crucibles were used to hold all melts except those containing zirconium, for which zirconia crucibles were necessary. Temperatures were measured by a disappearing-filament type optical pyrometer sighted vertically downward on the melt surface through a 1/4-in.-diameter sight hole in the crucible lid. By means of a technique previously described, 9 in which the refractory-metal nitride was precipitated at one temperature then redis-solved by raising the temperature 50°C and precipitated again at a higher temperature, it was possible to obtain data over a temperature range of up to 200°C on a single melt. It was found that this technique could not be used with melts containing zir-

Jan 1, 1965

By Raynor Linzey, Karl M. Busen

The formation of thin films of silicon oxide by anodic oxidation of silicon and the subsequent removal of these films by an etch is a process often used for the evaluation of concentration distributions Profiles) in silicon layers by the differential sheet conductance method. The accuracy of the resulting profile is very strongly influenced by the uniformity of the thickness of the reacted silicon. Normally, it would be expected that for a constant number of coulombs passed the thickness would be the same from oxidation to oxidation. Investigations show that in certain electrolytes, for a given number of coulombs passed through an n-type silicon sample, the thickness of the reacted silicon increased with increasing resistivity. Even for the same resistivity the thickness varied sometimes by a factor of 1.5. When an electrolyte was used which consisted of 10 pct water by volume in ethylene glycol with 4.0 g KNO per 1000 ml of solution, anodiza-tion at 5 ma per sq cm led to satisfying results. Short-time anodizations gave oxide layers of a higher apparent density than those experienced from thermally gown silicon oxides. THE functioning and the electrical characteristics of semiconductor devices are based upon the incorporation of "impurities" into a single-crystalline body of suitable material and on the concentration distribution (profile) of this impurity. The incorporation can be achieved by well-known processes as, for example, by diffusion, epitaxial growth, alloying, or ion implantation. Often the profile resulting from these processes is not known. A powerful tool to learn about a concentration distribution is given by the method of differential sheet conductance which employs successive four-probe measurements on a layer subjected to stepwise removal of thin sublayers. Differential sheet conductance vs position (or penetration depth) of a sublayer is plotted and a smooth curve is drawn through the data. From this curve the profile is then calculated. When the semiconductor material is silicon, the sublayers are removed suitably by anodic oxidation of the silicon and subsequent dissolving of the formed silicon oxide by an etch. The accuracy of the resulting profile is very strongly influenced by the uniformity of the sublayer thickness. Normally, it would be expected that, for a constant number of coulombs passed, the thickness would be constant from oxidation to oxidation. Investigations showed that for sublayers several hundred angstroms thick the reproducibility can be rather poor. Therefore, efforts were made to obtain a reliable technique for uniform removal. The present paper describes such a technique and certain phenomena which were encountered during the investigations. APPARATUS AND TECHNIQUE The first report on the investigation of concentration distributions, where for differential sheet conductance measurements thin silicon sublayers were removed from a diffused layer by anodic oxidation, was given by Tannenbaum. The author reports the removal of sublayers which for the most part were 400 thick. More advanced device designs now require much narrower layers. When it was tried in these laboratories to determine profiles within such layers, difficulties were encountered with respect to sublayers which by necessity had to be thinner than the ones reported by Tannenbaum. The apparatus used for the investigations is sketched in Fig. 1. Two cylindrical containers connected by a wide tube are filled with an electrolyte. The left container receives the cathode whereas the right container is closed at the bottom end by a sample support consisting of a Teflon base and a copper pedestal. The silicon sample (1 by 1 cm) is mounted to the pedestal embedded flush in the Teflon base using silver paint (Degussa) for electrical contact. Pyseal is applied to the edges of the sample to protect the copper pedestal from the electrolyte. The base is mounted to the container using a water-tight silicon rubber gasket. Fig. 2 gives a view of the sample support. The copper pedestal is connected to the positive side of a power supply operating at a constant current output (Kepco Model ABC 425M). The electrolyte which has been reported by Duffek et al. consisted of either 2 or 10 pct water by volume in ethylene glycol and 4.0 g KNO3 in 1000-ml solution. The electrolyte is best prepared

Jan 1, 1967

By J. L. Dumanoir, Maurice Martin

The induction-electrical log is a combination of a SP curve, a short normal curve, and an induction log; all three logs being recorded simultaneously in a single run. The spacing of the short normal is 16 in. The induction log is designated as 5FF40, which means that the sonde involves five coils and a focusing system, and that the distance between the main coils is 40 in. Examples of induction-electrical logs are shown in Figs. 13 and 15. The right-hand track contains the induction conductivity curve. The scale of this curve is linear with the units of conductivity, i.e., mhos/m or millimhos/m (mmhos/m), increasing from right to left. The same curve can be read in the reverse direction as a resistivity log, with a hyperbolic scale. In the middle track, the solid curve represents the short normal. (An amplified short normal is also shown in Fig. 15). The dotted curve is the resistivity curve of the induction log, i.e., the reciprocal of the conductivity curve, recorded with the same linear scale as the short normal. The SP is in the left-hand track. In this combination, the SP curve and the 16-in. normal are the essential correlation curves, as in the conventional electrical log. The induction log provides a more accurate and detailed record of formation boundaries than the conventional log, especially in hard rock territories. Furthermore, the induction-electrical log makes possible the determination of fluid content, particularly in thin beds—at least qualitatively and very often quantitatively. In such thin beds, because of the adverse effect of the adjacent formations, the responses of the conventional devices are generally doubtful and/or incom-plete. Another advantage of the new combination is that the induction log is little affected by the presence of thin hard streaks interbedded within the permeable sections, whereas such occurrences are the cause of serious distortions of the long normal and lateral curves. The evaluation of saturation from any resistivity log implies the knowledge of the true resistivity R, of the bed and of the resistivity R.. of the flushed zone, or at least of the ratio Rxo/Rc. With the induction-electrical log run in fresh mud, the 16-in. nor-mal has a smaller radius of investigation than the induction log, so that the former reads closer to R.. and the latter closer to Rt. Thus, it has been observed that the ratio of the 16-in. normal to the induction log readings can be used as a basis for the interpretation in terms of saturation, with the help of appropriate charts. The purpose of the present paper is essentially to explain this procedure and to provide the corresponding charts. On the other hand, when a formation is deeply invaded, the response of any log (in particular the induction log) depends upon the radial distribution of formation resistivities behind the wall of the hole, which itself is a function of the arrangement of the fluids saturating the formation pore spaces. This paper, accordingly, will begin with a schematic description of the distribution of fluids and resistivities in the invaded zone. Next, some essential characteristics of the induction log will be reviewed. Finally, the determination of the interpretation charts and their application will be explained. The discussion will be confined to the case of fresh muds, i.e., muds whose resistivity is at least five times as great as that of the formation waters. With the present equipment the induction log is not well adapted for logging in salty mud. The Laterolog and guard electrode log are at their best under conditions of low resistivity mud. Accordingly, when these tools were introduced a few years ago, the use of salty mud was recommended. Now, with the introduction of induction logging, spe-

Jan 1, 1958