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By S. Ramachandran, N. J. Grant, T. B. King

MANY investigations of the rate of the sulfur transfer reaction between carbon-saturated iron and blast furnace type slags have been made." It is evident that the reaction is complex, the rate being affected by the presence of elements dissolved in the metal that are readily oxidized and therefore capable of existing in the slag phase. Thus Goldman, Derge, and Philbrook- have shown that carbon, silicon, manganese, and aluminum, in order of increasing effectiveness, accelerate sulfur transfer from iron containing these elements to blast furnace type slags. Quantitative information is still, however, not available on the relation between what have been termed side reactions, such as silicon transfer and CO evolution, and the sulfur transfer reaction itself. In other words, the stoichiometry of the reaction has not been investigated. In the present investigation, the transfer of all reacting elements and the evolution of CO have been measured simultaneously in order to establish the mechanism of the reaction which occurs in practice. Information of this nature cannot be deduced from equilibrium studies. It should be pointed out that in kinetic studies of this type quantitative conclusions are applicable only to the system studied. This restriction should be borne in mind when attempts are made to compare results from different investigations. Apparatus The apparatus used enables slag and metal samples to be taken at frequent intervals and also provides a continuous record of the amount of gas evolved. A sketch of the apparatus is given in Fig. 1. It may be considered in three sections: 1) furnace section, 2) blank volume section, and 3) pressure measuring section. The furnace section is shown in detail in Fig. 2. It consists of two graphite crucibles, C and D, super-

Jan 1, 1957

By C. E. Melbye

A serious problem confronted the city of Gunnison early in 1958 in that, for a few months during each spring runoff, the water supply derived from the Gunnison River became polluted to an unsafe point. The city management had the choice of building a new filter plant to replace the old unworkable one or drilling wells to develop a ground water supply. The cost of a new filter plant was estimated at $180,000 compared to $50,000 for 6 wells, pumps, and additional water lines, hence their decision to attempt the development of sufficient ground water. Six wells at 300 gpm per well were estimated as necessary to handle the peak usage of 1800 gpm, compared to only 600 gpm winter usage. Although the water table is only about 7 feet below the surface, existing private wells drilled at random locations were producing much less than 300 gpm. The problem was to find sufficient quantities from about 6 wells. Since the presence of an ancient bedrock channel was suspected, which would be expected to localize greater quantities of water, the city of Gunnison authorized a resistivity survey to investigate bedrock topography below unconsolidated gravels. Survey results were highly satisfactory and led to the preparation of a fairly detailed bedrock contour map, Fig. 1. This map was used in selection of all well sites. The city of Gunnison is situated in a flat, broad, Quaternary gravel-filled valley (terrain dips south at 20 feet per mile) at the junction of the Gunnison River and Tomichi Creek. The valley, about 2-4 miles wide, is bordered by hills of Tertiary volcanics to the northwest, Cretaceous and Jurassic sediments to the north and northeast, and pre-Cambrian granite and gneiss to the south. One previous deep test well at the west end of the city hit pre-Cambrian granite at 496 feet, which, allowing for 40 feet of surface gravels, makes the older sedimentary section 456 feet thick. This section is probably all Jurassic Morrison formation, consisting of the Saltwash sandstone overlain by the much thicker section of Brushy Basin shales and mudstones. According to the driller's logs, each well was bottomed in what is believed to be Brushy Basin shale. FIELD PROCEDURE A standard Gish-Rooney type of resistivity apparatus was employed, which used 45-volt dry batteries as a direct-current power source. Applied voltages could be selected from 45 volts to a 270-volt maximum. Copper-coated steel stakes were employed as current electrodes and porous porcelain pots as potential electrodes to avoid possible polarization effects with direct current. The expanding Wenner electrode configuration was utilized for this investigation and measurements were made at 20 40, 60, 80, and 100-foot spacings,

Jan 1, 1961

By G. H. Wigton

THE oxidized ores of the Chief Consolidated Mining Co., in the Tintic mining district, have never yielded to metallurgical treatment by any standard method except smelting. These ores occur in comparatively small, irregular, siliceous replacements in limestone, and carry silver, lead, and gold as the principal valuable metals. But smelting methods. are unsatisfactory, as the lead smelters heavily penalize the large amount of silica in the ore, and the copper smelters do not pay for the lead in the ore; therefore, an alternative treatment method was sought. In 1916, a metallurgical research department was organized under; the direction of the writer. Many standard metallurgical methods were investigated but, on oxidized ore, none yielded extraction great enough to make its use feasible. During some chloridizing-roasting experiments in 1916, made in an assay muffle, the writer noted that large proportions of the silver, lead, and gold were volatilized from certain oxidized ores. The possibility of volatilizing the metals and collecting them in the form of a concentrated fume was then studied. But, as it was shown that satisfactory chloride-volatilization would be limited to a furnace feed with a high fusing temperature of the non-volatilizable constituents, and as the results obtained in a rotary kiln with the admixture of common salt with the ground ore were inferior to muffle tests, further volatilization experiments were discontinued until 1920. During this interval, an experimental sulfidizing and flotation plant was operated. After the cessation of attempts to float the oxidized minerals, chloride-volatilization experiments were resumed. The highly infusible flotation. tailing from the operation of the flotation mill was used for furnace feed. The first tests made on flotation tailing mixed with 10 per cent. common salt showed -nearly complete lead and gold volatilization but considerably less volatilization of silver than in muffle tests. In attempts to increase the silver extraction, the percentage salt in the furnace feed was varied, and it soon became apparent that the use of smaller percentages of salt raised the fusion temperature of the furnace charge and thus,

Jan 8, 1925

By M. F. Trice

PYROPHYLLITE is a hydrous aluminum silicate (A12Si4010(OH)2)1 that occurs in both the foliated and the massive forms. The foliated variety resembles talc in that it has a greasy feel, a pearly luster, perfect basal cleavage, and usually is white, although in some deposits apple green, gray, brown, russet, and nearly black specimens may be found. The massive deposits of pyrophyllite yield pearl gray to light tan aggregates, some of which are so friable that they may be crushed with the hands into a fine gritty powder. Frequently specimens of the massive variety are studded with crystals of radial structure. The mineral has a specific gravity of about 2.7 and a hardness of 1 on Mobs' scale.1 The chemical composition of commercial pyrophyllite reflects the mineralogy of the deposits, which, according to Stuckey,2 contain pyro-phyllite and quartz, together with chloritoid, sericite, and a few other minerals of negligible importance. The latter, he says, "are noticed in but small quantities to the extent they might occur as accessory constitu-ents of an igneous rock or as products of regional metamorphism or weathering. . . . Quartz is abundant everywhere except in the very best grades of pyrophyllite." Analyses of specimens from several deposits are listed in Table 1, showing that the silica content varies from 57 to 73 percent and the alumina from 22 to 33 percent. Oxides of iron and the alkaline metals are collectively present, with one exception, to an extent of about 1 to 1.5 per cent.

Jan 1, 1940

By E. B. Johnson

Cleveland-Cliffs lron Co., which operates Marquette lron Mining Co.'s Republic mine, conducted a test whereby 35,000 tons of self-fluxed pellets were produced in the grate-kiln system from specular hematite flotation concentrates. A brief description of the pelletizing plant is presented along with pertinent operating details. Date is included which compare operating conditions and the chemical and physical properties of the green and fired pellets for the self-fluxing pelletizing test with the normal acid pelletizing operation. The success of self-fluxed sinter in enhancing the operation of the blast furnace during the past few years has reasonably led to the assumption that the use of self-fluxed pellets might result in even greater furnace efficiencies. A great share of development work in agglomeration has been directed towards techniques related to the production of self-fluxed pellets, but only a limited tonnage of self-fluxed pellets had been produced on a commercial scale until this past year when The Cleveland-Cliffs Iron Co. produced 35,000 tons of such pellets by the grate kiln system at the Republic mine during the period May 21-June 5, 1962. REPUBLIC'S GRATE-KILN PLANT The grate-kiln pelletizing process consists of four stages, namely: feed or balling circuit, traveling grate, rotary kiln and annular cooler (Fig. 1). The balling section is conventional and utilizes four 9x30-ft balling drums in closed circuit with 5x14-ft vibrating screens having 3/8-in. rod decks. The traveling grate is 12 ft wide by 126 ft long and has 14 windboxes — six in the drying section and eight in the preheat section. The rotary kiln is 15 ft ID shell and 114 ft long. The annular cooler is 40 ft in diameter and has 12 windboxes. The cooler is divided into two zones by a moveable curtain wall. The high temperature air from the first zone is used as secondary combustion air in the kiln. Normally the only heat supplied is through the burning of No. 6 oil in the single kiln burner. Hot gases pass counter to the pellet flow through the system. The exit gases from the kiln pass down draft through the preheat section through cyclones and are drawn through the drying bed prior to exiting via the stack. The temperatures are normally held within the following ranges: Kiln 2400-2445 °F Preheat 1850-1950°F Drying 480-520°F Exit gas 200°F Pellets 120°F The design capacity of the Republic mine grate-kiln system was 2500 Itpd. Sustained production in excess of 35% over design capacity has been achieved. No screening of the cooler product is practiced. PELLETIZING TEST CONDITIONS When a decision was made to proceed with a test at the Republic mine pelletizing plant to produce 35,000 tons of self-fluxed pellets, several potential failure factors had to be carefully considered. Research work on a batch and pilot plant scale indicated that the grate-kiln system at Republic would require some major changes in order to obtain optimum conditions. In many cases compromises were agreed upon as major equipment changes and revisions were not feasible. The pelletizing conditions which laboratory development tests revealed were required in order to insure successful production of self-fluxed pellets were: 1) Good mixing of limestone and concentrate and proper moisture control; 2) Higher gas flow rates in the preheat section than are normally used; 3) Higher preheat temperatures than normal; 4) Maximum kiln temperature 2350°F. There was just cause for concern about balling problems that might occur. Approximately 10% of dry pulverized limestone was to be added to the specular hematite concentrate just ahead of the Pekay mixers on the belt feeding the balling drum. Large scale

Jan 1, 1963

Jan 1, 1966

By David C. Jonson, W. Bruce MacKenzie, Arthur A. Bookstrom, Vaughn E. Surface, Neil K. Muncaster, Stewart R. Wallace

In mid-Tertiary time a wet silici-alkalic magma penetrated the Precambrian rocks of what is now the Tenmile Range of Central Colorado and formed the Climax Stock. The stock is a composite one and was intruded in four separate irruptions, each giving rise to a major hydrothermal event. The first three of these produced large stockwork ore bodies that cap and flank the tops of their respective source intrusives; the fourth, and last, yielded almost no commercial mineralization. The ore bodies and their related zones of alteration are circular to ring-shaped in plan and arcuate in section. The different phases of the stock are so positioned with respect to each other that many of the circular and arcuate zones of mineralization and alteration overlap or are juxtaposed. Evidence of a time separation between the different ore bodies is found in certain dikes that were intruded between periods of mineralization and are well mineralized in one ore body but are barren in another. If it is assumed that the parent magma at Climax contained 10 per cent "water," that the "water" contained 0.1 grams per liter of molybdenum, and that the processes of extraction were 100 per cent efficient, then approximately 10 cubic miles of magma would be required for the formation of each ore body. The volume requirements, taken in conjunction with the cross-sectional areas of the different phases of the stock to explored depths, suggest to the authors that each magma chamber was columnar, extended to a depth of thousands of feet, and was connected with a much larger master reservoir. The repetition of similar intrusive, structural, and hydrothermal events, indicates periodic tapping of this reservoir. A regular chemical evolution of the parent magma is suggested by the systematic change in metal ratios and differences in the sites of deposition, relative to the source intrusive, in each of the four separate igneous hydrothermal stages. The preparation of ground was due to changes in magmatic and/ or hydrothermal pressures within the igneous-hydrothermal columns; small, repeated, up and down movements of the rock enclosing the tops of the columns formed the stockwork fractures into which the mineralizers penetrated. The forceful emplacement of each successive phase of the Climax Stock resulted in a slight doming and rotation to the westward of the earlier-formed geologic features. Postore normal displacement along the Mosquito fault is estimated at about 9000 feet. Part of one ore body was cut by the fault and lies at depth below the Paleozoic sedimentary strata on the hanging wall. On the footwall side of the fault, subaerial erosion and glaciation removed a large part of one ore body and uncovered the top of a second.

Jan 1, 1968

Jan 1, 1966

By W. V. Long, D. H. Reynolds, R. B. Bhappu

Equilibrium distribution coefficients were determined for some monovalent and polyvalent ions for several absorbing and exchanging media as functions of pH and initial ion concentration. Among ions studied were NH4 (I), K(I), Ni(II), Ce(III), Th(IV), and Mo(VI). Absorbents used were: ion exchange resins; a tertiary, and a quaternary amine in an inert solvent; and some activated carbons. The ions studied were in aqueous HCI, HNO3, H2SO4, or HC104 solutions. The classical mass action expression proved of little value in describing the variations observed. The data indicate that the determining factors in absorption and ion exchange may be the ionic species in the aqueous solution, which in turn depend upon pH, dilution, and perhaps other conditions. Three sorption processes have become prominent in recovering values from leach solutions. These are: 1) ion exchange, 2) solvent extraction (liquid ion exchange), and 3) physical adsorption by materials of high specific surface. In the first two of these processes the exchange reaction is considered chemical in nature, and is discussed in terms of the mass action principle. The third is considered a surface phenomenon and is discussed in terms of surface areas and various forms (Gouy, Stern, Grahame, etc.) of the Helmholtz double-layer theory. Generally speaking, we have found in chemical analysis and hydrometallurgical studies that there are close similarities between the three sorption processes, and also differences which are difficult to reconcile with any of the usual theoretical treatments. That others have experienced the same troubles is shown by the fact that usable processes, in chemical analysis as well as in hydrometallurgy, generally are discovered by empirical procedures. EXPERIMENTAL CONSlDERATlONS The gaps between theory and practice have allowed many conflicting statements to appear in the litera- ture. To learn, in particular, the behavior of some metallic ions on a cation exchange resin at a constant pH, equilibration studies were made over a wide range of concentrations.' Results are shown in Fig. 1 for four metals in hydrochloric acid solution on a strongly acidic cation exchange resin, AG 50W-X8 (Bio-Rad). The distribution coefficient, defined as D = amount of metal extracted per g of resin/amount of metal unextracted per ml of solution is seen to vary in a way to support all manner of reports about its behavior with changes in solution concentration. The metals used were chosen from those least likely to form stable chloro-complexes. The changes of slope in the various isotherms may reflect formation of unsuspected chloro-complexes of low stability (ion-pairing for example) whose concen-

Jan 1, 1967

By M. R. TECK, N. Rudd, L. K. Thomas, D. L. Katz

The authors are to be congratulated for presenting the first comprehensive paper on the theory and practice of threshold pressure determination in connection with underground gas storage. It is of particular value since most previous experimental work on this subject has been proprietary to the commercial laboratories engaged in such testing and to their clients. This dlscussion is presented in amplification of the subject paper, not in criticism, and is based upon our experience with approximately 5,000 threshold pressure determinations. Our comments are directed primarily to the experimental procedures as described by Thomas et al. It should be noted that, while clay mineral-rich lithologies are the most common caprock materials, the samples used (Table 1) include low permeability sandstones and carbonates, but do not include shales or other formations in which clav minerals exert a dominant effect. While our experience on samples analogous to those investigated by the authors generally confirms their findings, we have found that even more rigorous experimental conditions must be imposed where clay minerals are the controlling factor. These additional conditions result from the well-known molecular character of the clay minerals themselves in which water is interlaminated with, and bonded to, silicate sheets, thus becoming an essential component of the molecule. In many clay minerals the character of the intersheet bonding, and thus the dimension of the lattice, is strongly affected by variations in the identity and concentration of cations present in the intersilicate water. On a supermolecular scale, adsorbed water films on particle or "flakes" of shale provide much of the cohesive force necessary to maintain mechanical strength. The thickness of these films is variable and inversely proportional to intergranular pressure within the dimensional limits involved in caprock investigation. The thickness of the intersilicate water layers may also be subject to pressure under some conditions. These considerations are reflected in several necessary modifications of the experimental procedures described by the authors. Two of these are, in our judgment and experience, of such importance that they cast real doubt on the validity of data obtained on argillaceous materials without their application. The very careful resaturation procedures proposed by the authors should give good results in connection with the relatively "inert" lithologies used in their experiments. Our experience suggests, however, that they would create more problems than they would eliminate if applied to argillaceous materials. 1. Drying of the sample at the temperature and for the duration indicated by the authors not only will dessicate the sample with consequent shrinkage cracking, parting along bedding planes, and even total disassociation in the case of fissile shales, but it may also alter the character of the clay minerals themselves — in some cases irreversibly. 2. Prolonged evacuation to 2 microns Hg further dessicates the sample and is even more effective in reducing the intersilicate water content. 3. Resaturation with water differing in pH or chemical content from that existing originally in the sample also serves to alter the nature of the sample, particularly its structure and strength. 4. Our experience has been that, even with the thorough precautions proposed by the authors, complete resaturation of very fine grained materials is rarely obtained. Yet our experience confirms the

Jan 1, 1969

In 1962, minerals beneficiation showed definite signs of coming out of the doldrums into which it has drifted after the uranium boom. Demand by steelmakers for high-grade iron pellets has created the need for concentrating plants to upgrade specular hematite by spiral concentration or flotation and magnetites by magnetic means and flotation. According to a paper given at the AMC annual meeting by C. S. Arms of Pickands Mather, "the shipment of pellets, started in the mid-1950's, has increased to 17.6 million tons in 1961 from North American operations. Many plants already underway will raise this production to about 42 million tons by 1965. This will be a very sizeable percentage of the total iron ore production contemplated by that date." Iron ore concentration methods are gradually raising the assay of pellets into the 65 to 69% Fe range and lowering silica to the 4 to 7% range. Quebec Cartier's Lac Jeannine concentrator went into operation in late 1961 and all grinding units were running by 1962. The Iron Ore Co. of Canada's new Carol Lake plant was started in mid-1962.

Jan 2, 1963

Jan 1, 1969

By K. C. Mills, E. T. Turkdogan

A number of investigators1 6 have noted the presence of a liquid miscibility gap in the Fe-Sn binary system. However, the first attempt to measure the

Jan 1, 1964

By P. O. Metz, E. L. Wiehe, J. S. Foster

BASED on their analyses of growth kinetics, ibbs' and Harris et al.' have recently proposed that the rate of subcritical graphitization of steel is controlled by the rate of diffusion of carbon in ferrite. illert has concluded that this is the rate controlling growth mechanism when the growing graphite particles are relatively large. Harris et al.' also propose that the matrix surrounding a growing graphite particle is plastically deformed to make room for the growing particle. If this plastic deformation does occur, then preferred recrystallization may be observed around the larger particles. If diffusion of carbon in ferrite is rate controlling, then a graphite particle growing in a matrix of, say, tempered martensite or pearlite, should be surrounded by a carbide depleted zone. Thus, the simple metallographic experiments reported here are sufficient to determine whether or not diffusion of carbon in ferrite is the dominant mechanism for the growth of graphite in steel. The present investigation considers graphitization in five alloys. The compositions are given in Table I. Graphitization was carried out at three temperatures: 900°K (627"C), 950°K (677"C), and 990°K ('717°C). Samples were reacted in both the martensitic and the pearlitic initial conditions. In the hypoeutectoid steels, Sets 7 and 8, .and in the hypereutectoid Fe-C binary, Set 6, graphitization was very limited after 1000 hr at temperature. In these samples graphite particles observed were less than 10 p in diam. In the hypereutectoid commercial steels, Sets 1 and 3, large graphite particles (100 p) did not appear until after 250 hr at temperature. The limited number of graphite particles observed and the range of sizes obtained prohibited measurement of growth rates in this investigation. However, in all samples showing graphitization, neithe a carbide depleted zone nor recrystallization was observed. illert's model predicts that diffusion of carbon in ferrite should become dominant for graphite particles larger than about 300 p in diam. The largest graphite particle observed in this investigation was approximately 450 p in diam. No evidence of carbide depletion was noted. Fig. 1 shows a typical graphite particle. This nodule is from an initially pearlitic sample from Set 3 after

Jan 1, 1970

By W. D. Johnston, T. P. Thayer

THE minerals that collectively are known as chromite form an isomorphous series of the general formula (Mg,Fe) 0. (Cr,Al,Fe) 203. So wide is the range in chemical composition in this group that chrome ore consisting entirely of the mineral chromite may range from less than 30 pct to more than 60 pct Cr203. The most comprehensive published data on the chemical com- position of chromite are by Stevens,62 who made complete analyses of 52 samples of chromite concentrate from many localities in North, Cen- [ ] tral, and South America. These samples were mechanically purified to remove associated silicates and might be regarded as the cleanest chromite that could be obtained by any mechanical milling process. Fig 1 shows the predominant zone of isomorphism, within the triangular prism of composition defined by the mineralogical end members of the series, wherein his analyzed samples fell.

Jan 1, 1949

By R. L. Fullman, J. W. Cahn

A method is derived for obtaining the distribution of sphere diameters and plate thicknesses (or pearlite spacings) from size distribution functions obtained along randomly oriented lines. The method described offers several advantages over existing methods. IT is often of interest to measure not only the average particle size but also the distribution in sizes of particles dispersed in an opaque material, such as an alloy. Particles of a single size will exhibit a range of apparent sizes on the plane of polish. If the sample contains a distribution of particle sizes, the distribution of observed sizes on the plane of polish is related to the distribution of actual particle sizes by an integral equation, For example, a distribution of sphere sizes, N(r),

Jan 1, 1957

By Ogden Malin

IN conducting the manufacture of extruded brass rods and brass forgings it has been noticed that there is considerable variation in the physical properties, particularly the machinability of different rods and forgings, even though the composition, working temperatures and method of manufacture remain the same. It is the purpose of this paper to attempt to establish the cause and extent of this variation, and also to determine whether variations in composition within certain defined limits influence hardness and machinability to any marked degree. The writer believes that this variation probably is due to the variation in grain size of the metal, therefore the microstructure of several compositions under various conditions of working were examined in an effort to establish this as a fact.

Jan 1, 1932

By P. G. Hallof

Only recently has the term Induced Polarization found its way into geophysical literature. Schlumberger first mentioned the possible use of the induced polarization effect in one of his early papers. Later, induced polarization was the subject of several university theses, such as Seigel's at the University of Toronto and Bliel's at the Michigan School of Technology. In addition, a group at the New Mexico School of Mining and Technobgy has done work on induced polarization. There is very little to be found in print on the subject of induced polarization. Several papers have been presented at meetings, the 1958 AIME and SEG* conventions, for instance, on laboratory measurements of the effect and theoretical considerations useful in the interpretation of field results. This paper is the first attempt to present actual field results which show the usefulness of induced polarization as a prospecting technique. There are several phenomena that can cause polarization when electrical current is passed through the ground. In a paper presented at the 1958 SEG* meetings Professor T. R. Madden of M. I. T. demonstrated that only two of these gave rise to appreciable effects. The first is a result of the membrane and diffusion effects in a sandstone that contains appre- ciable amounts of clay minerals. The unbonded charges associated with the clay mineral forma material that passes positive and negative ions with different mobilities. When current is passed through such a system for some period of time, polarization results. The second phenomenon, which gives rise to very much larger polarization effects, is the one used in the new prospecting technique. These effects are a result of the blocking action or polarization of metallic or electronic conductors in a medium of ionic solution conduction. This electrochemical polarization, called "the over-voltage effect" by electro-chemists, occurs whenever electrical current is passed through a volume of rock which contains metallic minerals such as base metal sulphides. This polarization at metallic interfaces in ionic solutions depends upon the chemical energies necessary to allow the ions to continue the flow of current by giving up or receiving an electron from the metallic surfaces. The energy stored in this reaction isanalogous to that stored when a condenser is charged. If a d. c. current flowing through such a system is interrupted, the polarization can be detected as a small, decaying current that flows after the applied current is discontinued. The decaying potential measured is a result of the current flow caused by charges returning to their equilibrium positions from the positions they assumed under the applied potential field. Because of the polarization, there is an excess of change at each metallic interface. There is an alternate method of measurement of the induced polarization effect. The electrical

Jan 1, 1961

By K. E. Manchester, C. B. Sibley

The feasibility of doping silicon to produce device structres by directly implanting impurity atoms has been demonstrated. Both phosphors and boron ions have been successfully implanted in silicon to produce electrical junctions. Junctions as deep as 1.2 p have been produced by phosphorus ions having energies the order of 80 kev. An electromagnetic separator has been used to controllably produce uniform, large-area implantations for evaluation experimentation. Correlations between junclion depths and ion energies huve been obtained. Orientation effects have been observed and it has been found that the (110) direction is the easy direction for implanting. Monitoring of thermal treatments oj implanted substrates by sheet-resistance measurement indicates a very mild thermal anneal removes most of the damage done during the implantation. These indications are further substantiated by reverse-current measurements of j,inctions Produced by implantation. Electrical characteristics of implanted junctions are compared with those of diffused junctions. We have been interi n the interaction of energetic ions in the III-V groups, in particular boron and phosphorus, with single-crystal silicon to produce type conversion for possible device use. A number of investigators, a few of whom are avies, Kornelson,3 and so forth, have reported on penetration of energetic ions into both amorphous and crystalline solids. While most work has been done with ions of the rare gas and alkali metal groups, some work has been reported by ing, erber,' and others6 in which ions of the 111-V groups have been implanted in single-crystal silicon. A large amount of this work has been done with ion energies in the 100-kev to 1.5-Mev range. An excellent review article has been written by caldin. We have concentrated on ion energies which are in the 10 to 80 kev range, with which over 1500 implanted junctions such as the one shown in Fig. 1 have been produced in silicon substrates with both phosphorus and boron ions. Fig. 1 is a 3-deg angle lap in which the n type area produced by 66 kev P is delineated and the junction is 9500A below the surface. EXPERIMENTAL Implantations reported in this paper were made with the ion source adjusted to produce ion currents in the range of 1 to 2 pa with accelerating voltages varied from 10 to 40 kv. When using doubly charged ions this produced 10 to 80 kev ions. This allowed substrate temperatures to remain below 100°C. Sam- ple movement resulted in beam impingement angle variation of 7 deg from the normal to the substrate surface. Substrate resistivities have been varied through the range of 0.001 to 500 ohm-cm and specimens oriented in three directions, (110), (Ill), and (loo), within 12 deg. RESULTS For the purpose of this paper, discussion of results will be limited to phosphorus implantations with mention of results for boron-implanted silicon. Similar results have been obtained for boron and will be reported at a later date. In Figs. 2, 3, and 4 depth penetration is shown

Jan 1, 1967

By C. G. Dunn, P. K. Koh

The primary recrystallization textures of 11 single crystals cold rolled 70 pct were determined. The effect of crystal orientation on recrystallization behavior was investigated also and found to be large. An exception was found to the relationship that strong components of the recrystolliza-tion texture are rotated from the cold rolled texture by 30° about <110> axes, but generally this relationship was found to hold quite well. Evidence supporting oriented nucleotion was found and discussed in terms of probable active slip systems and <110> edge dislocations. THE present paper is one of a series&apos;.&apos; on recrys-tallization phenomena in cold rolled 31/4 Si-Fe single crystals and is mainly concerned with the textures produced on recrystallizing from stable end orientations. Data for the cold rolled textures of the crystals used have been reported by Koh and Dunn." Their results showed that the sharpness of the cold rolled textures varied throughout the range of stable end orientations and that the tendency to re-crystallize was related to the sharpness of the cold rolled texture, wherein the rate of recrystallization increased and the size of recrystallization grains decreased with decreasing sharpness of the cold rolled texture. In the project under consideration the cold rolled crystals involved a range of initial orientations that, together with those studied earlier,&apos; provide information on several points. The first point is whether the recrystallization texture from a (111) [112] cold rolled texture, a stable end orientation that can be approached from different directions, correlates in any way with the initial orientation before cold rolling, or whether the recrystallization texture is entirely determined by the observable features of the cold rolled texture. The second point involves a preliminary study to see if the main components of the recrystallization textures correlate with the most probable active slip systems. The third point is to determine what effect departure from slip on one slip system has on the tendency to recrystallize. Experimental Procedure Nine specimens from a previous investigation and two additional ones from thicker stock (lot D) but of similar composition to the others were used in the present work. The latter two crystals, like the nine, were cold rolled to a reduction in thickness of 70 pct and the amount of widening was determined. Depending on their primary recrystallization behavior, the cold rolled crystals were given short or long anneals at temperatures of 980°C or higher. Table I summarizes the data on initial orientations, the textures obtained by cold rolling, and the anneals given to provide samples for the present work. Fine grained specimens were thinned to 0.002 in. thickness and placed in an integrating specimen holder. Chart recordings using a transmission X-ray method and MoKa radiation were obtained for diffraction from (110) planes. This method,&apos;,3 which gives data for all of the pole figure except a central region of 30" radius, proved sufficient to give generally five, and sometimes six, of the six possible pole concentration areas of any one component of the texture. These data, therefore, were generally adequate for a positive identification of each component present. The first texture obtained for specimen B-2 was poorly defined because of too coarse a grain structure and therefore too few crystals in each component for satisfactory X-ray reflections. The same

Jan 1, 1957