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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 V. Taylor

"THE petroleum industry in Canada has been experiencing considerable difficulty in filling its manpower requirements during the last few years, and because of the rapidly expanding nature of the industry it is concerned about the supply that will be available to fill the needs of the future. As the oil industry is one of the more technically oriented industries, the most acute problem exists primarily in the field of profession-al/technical personnel. This is particularly true in the production and exploration side of the business, because it employs the highest percentage of this type of personnel. Let me illustrate this by giving you some figures reported by the Alberta Bureau of Statistics as of December, 1965 -out of a total of 9,641 male employees engaged in oil producing and geological and geophysical operations in Alberta, 3,021, or 31 per cent, were classified as engineers, geologists, geophysicists, managers and other professional personnel. No figures are available for 1946 to make a direct comparison of the expansion of the industry over the past twenty 466 years, but it is doubtful whether more than 100 professional/technical people were engaged in producing in Alberta at that time"

Jan 1, 1967

By Erle C. Donaldson

The pendant drop interfacial tensiometer is being used to study interfacial phenomena that influence the production of crude oil. A description of the instrument showing the modification of the cell and cell holder is presented. The modified cell and cell holder allow formation of a precise and reproducible drop size, and the image of the drop is easily alined and focused. Interfacial tension measurements and observations of film formation can be conducted at various temperatures with the jacketed cell.

Jan 1, 1967

By Ronald L. Haxby

This report presents a refractive seismic technique for evaluating the strength of rock within an open pit bench. A concept of correlating rock strength and seismic velocity is discussed and a method of predicting the degree of fragmentation of a pit bench is introduced, Figure 1 shows the area of interests [ ] Most of the work was performed while completing graduate studies at the University of Arizona.

Jan 1, 1967

By Murray Weintraub

In an investigation of the incineration of combustible wastes, the Bureau of Mines studied the effect of dimensional parameters, process variables, and fuel properties on the operation of an incinerator that consisted of a single cylindrical combustion chamber in which all combustion air was supplied tangentially above the fuel. Construction and operation of three designs of such a device proved that the tangential overfire air design is effective in providing efficient combustion and low concentration of particulate matter in the effluent gas. A correlation was found that related burning rate with air rate, chamber diameter, and inlet port diameter. In one of the incinerator models, ignition was by radiation from a preheated surface. The temperature of this surface was required to be 1,400° to 1,600° F to insure ignition of moist refuse; however, this had little effect on combustion rates. In the combustion of moist refuse, evaporation of the water proceeded through the fuel bed as a wave, with an ignition wave following the evaporation.

Jan 1, 1967

By Henry M. Harris

A study was made by the Bureau of Mines to determine if shapes of oxide-glass compositions could be roll-formed at high temperatures, and to find the conditions required for adequate formability. A unit with directly connect' furnaces and heated rolls that allowed forming of most of the compositions developed. Glasses of the feldspar type were chemically unreactive with the alumina grains, and allowed the best roll forming. Optimum forming was attained at temperatures of 1,400° to 1,530° C, with compositions containing 30 or 40 percent feldspar and 60 or 70 percent alumina. Formability was better when compositions contained minus 325-mesh materials, rather than coarser or finer powders. In many cases, roll-formed shapes had physical properties equal to or better than the normally sintered shapes of the same composition.

Jan 1, 1967

By Frank A. Peters

An evaluation is made of a lime-soda sinter process for extracting alumina from clay. In this process, alumina is extracted by sintering clay with soda ash and limestone and then leaching the sinter with a dilute sodium carbonate solution. The sodium aluminate solution formed during leaching is separated from the residue and treated with lime in autoclaves to remove dissolved silica before alumina trihydrate is precipitated with carbon dioxide. The tri-hydrate is then calcined to a-alumina. Two options, dry grinding and wet grinding, are used in the sintering step. The fixed capital costs for plants producing 1,000 tons of alumina per day are $72 million for the dry grinding option and $66 million for the wet grinding option on a Marshall and Stevens chemical equipment index basis of 240.0. Specific geographic locations of plant and raw material sources are not assigned, but, since this process requires large quantities of both lime-stone and clay, the plant site is considered as variable with relation to the clay mine and limestone quarry. A nomograph is given to find operating costs at various delivered costs of clay and limestone. If the plant is located nearer the limestone quarry so that the delivered cost of clay is $2 per ton and the delivered cost of limestone is $1 per ton, the operating costs are $76.47 and $71.61 per ton of alumina for the dry grinding and wet grinding options, respectively. On the other hand, if the plant is located nearer the clay mine so that the delivered cost of clay is $1 per ton and the delivered cost of limestone is $2 per ton, the operating costs are $80.15 for dry grinding and $75.34 for wet grinding.

Jan 1, 1967

By R. Priestner, R. F. Krause

Solid, cylindrical crystals of a iron have been fractured at 10°K by the simultaneous application of tension and torsion stresses. Thus, a complex distribution of normal (sN) and shear (ss) stresses existed in a cleavage plane at fracture. In every crystal the clearage-plane normal was inclined to the specimen axis, so that a unique point, M*, in the operative cleavage plane was defined where the quantities sn and s2 N + s2 S) were maximized. It is shown that the maxirrzum resolved normal stress on the cleavage plane at fracture decreased as the resolved shear stress in the cleavage plane at M* increased. Thus, a normal stress la?*! for fracture was not satisfied. A fracture law which takes shear stress into account. and which predicts that (s2 N +s2S) should be constant, is to be preferred. However, the data is best represented by a linear dependence of sN on sS, sS which 110 physical significance can be attached. It is suggested that the fracture-nucleating -mechanism is a short-range one. A critical stress law has not yet been unequivocally established for the propagation of cracks in metals. Measurements of the tensile fracture stresses of variously oriented zinc single crystals1 failed to establish the normal stress law expressed by In Eq. [1], sN is the fracture stress, P, resolved normal to the fracture plane, and 0 is the angle between the fracture -plane normal and the stress axis. Similarly, a comprehensive investigation failed to verify the normal stress law for the tensile fracture of a-iron single crystals.' However, a subsequent investigation,3 using iron from the same ingot, presented fracture data which obeyed the normal stress law. It has been shown previously4,5 that the Griffith criterion for fracture6 does not predict such a normal stress law. This result is of particular significance in considering the fracture of metals, such as zinc and iron, which may fail by cleavage. In these metals fracture propagates in a well-defined "cleavage" plane, whether or not an applied stress is normal to it. When the cleavage-plane normal deviates from the direction of application of a uniaxial stress, for example, the crack propagates under the combined action of normal (sN) and shear (ss) stresses. When the presence of a resolved shear stress in the crack plane is taken into account, the Griffith criterion is expressed by4

Jan 1, 1967

By Matthew J. Sheridan

The Bureau of Mines study described in this report was conducted in the Denver, Colo., area (1) to summarize existing conservation practices as related to the most beneficial utilization of deposits of sand and gravel; (2) to identify the conflicting positions of the aggregate producer, the mineral owner, nearby residents, and local government officials responsible for determining land status and for issuing operating permits; and (3) to show the need for planning in Denver and in other expanding communities toward obtaining the benefits of conservation of our rapidly dwindling mineral resources. In order to determine the effects of urbanization on the Denver aggregate industry, interviews were held with owners of sand and gravel operations, with producers of concrete and bituminous pavement, with city and county planning and zoning personnel, and with representatives of various interested organizations. The conservation and ultimate utilization of deposits of construction raw materials near expanding urban areas can best be accomplished by long-range land-use projection and the requesite cooperation of technically advised planning and zoning administrators, government officials, mineral producers, and land developers.

Jan 1, 1967

By J. B. F. Champlin

The continuing development of the nuclear industry in the United States requires a program of waste disposal that insures against the release of large amounts of radioactivity to the environment. This paper describes research on one proposed means of disposal of this waste, that of injection into geologic formations at depth. Nuclear production plant wastes were simulated and injected into samples of sedimentary rock obtained from outcrops, quarries, and deep wells. Changes in the chemical and physical characteristics of the rocks caused by the interaction of ions and suspended particles in the waste solutions with the cementing material and claylike particles in the rock are discussed. Laboratory tests show that nuclear wastes can be injected into many natural porous, permeable geologic formations. Injectivity can be maintained over a longer period by monitoring the ionic balance and particle-size distribution of waste streams. The combination of permeability and porosity with low cation-retention capacity, as exhibited by most sandstones, would satisfy the engineering requirements for the subsurface disposal of nuclear waste. Shales and clays with their low permeability and high cation-retention capacity would make excellent confining formations. The amount of cation retained by sedimentary rocks increases with increasing valence or concentration of the cation or decreasing brine concentration. The use of rock cores as model reservoirs had proved successful in determining some of the parameters that need to be considered in full-scale field disposal of wastes.

Jan 1, 1967

By C. M. Sellars, F. Maak

Electvomotie -force measurements hazle been made on ten Au-Ni alloys at temperatures 7754 825O, 900O, and 935°C using galvanic cells with solid electrolyte. Partial and ivtegral thermodynamic functions are derived from the determined activities. which show la9,ge positive deviations jvom Raoult's law. The enthalpies of mixing- are in close accord with calorinletric data and are of comparable accuracy. The results are used to determine the miscibility gap and the spinoidal curL1e, and are qlalitaticely interpreted in terms of the large size difference and electvonic interactions between gold and nickel. Tabulated nalues of the actielities and partial and inteqal free energies, entropies , and enthalpies of mixing are given in the appendix. The Au-Ni binary alloys are of particular interest thermodynamically as despite the large size difference between gold and nickel atoms they have a simple phase diagram.' This shows complete solid solubility above a miscibility gap with a maximum at about 71 at. pct Ni and 810°C. Activity measurements (over a range of temperature) have been made previously on this system using an electrolytic-cell method with a liquid chloride eletrolyte. The accuracy of this data has, however, been queried3'4 as it leads to values for the enthalpy of mixing which are too high when compared with calorimetric measurements.46 Also, the entropy of mixing is too high when compared with the values derived from specific-heat measrements. It was therefore considered worthwhile redetermining the activity data using a galvanic cell with a solid electrolyte (0.85 ZrO, 0.15 CaO). This method is based on a technique introduced by Kiukkola and aner'' and has been used to determine the thermodynamic data for Cu-Ni alloys.' THE ELECTROLYTIC CELL The cell used to determine the activity of nickel in Au-Ni alloys was: The cell reaction, which is discussed for a similar cell by Rapp and Maak, gives a direct measurement of the activity of nickel in the alloys as where aNi(alloy) is the activity of nickel in the alloy, 3 is Faraday's constant, E is the measured electromotive force, R is the gas constant, and T is absolute temperature. For the valid application of this type of cell the arrangement must be ther modynamic ally stable, which means that: 1) The free energies of formation of the oxides fulfill the relation 2) The vapor pressures or dissociation pressures of each component must be so small that during the time of the experiment the amount of any material transported by the gas is negligible. 3) Side reactions which change the alloy composition must be negligible. These reactions are possible both with the surrounding gas atmosphere and with neighboring solid material. The first two conditions are fulfilled by the above cell.' The third condition is approached by care in the experimental technique. The factors which control the attainment of equilibrium in this type of cell have been considered by Rapp and aak, who conclude that metallic diffusion in the alloy is the rate-control ling step. A lower temperature limit for the practical application of this cell is therefore set by the condition that equilibrium must be attained in reasonable times. EXPERIMENTAL MATERIALS AND TECHNIQUE The starting materials were mint gold (99.99 pct Au) and Mond nickel (99.9 pct Ni). Alloys, nominally 5 at. pct Ni and then each 10 at. pct across the system, were produced by vacuum-levitation melting compacts of mixed drillings of the pure metals. The nickel used for the reference tablets in the cells was melted in a similar manner. The alloy ingots, cast in boron nitride molds, were cold-forged and

Jan 1, 1967

By D. W. Bacon

Plant process optimization programs are often costly, both in technical effort and loss of production. Evolutionary Operation or "EVOP" is a mode of plant operation consisting of controlled cyclical changes in process conditions by which information is provided concerning potential process improvements while both volume and quality uniformity in production are maintained. Its conceptual simplicity and low cost of utilization have led to successful adoption in a variety of industrial manufacturing operations. This paper is an expository account of basic EVOP theory, the problems encountered and the organization required in applying it to a processing plant. Illustrations are provided which indicate the payoff that can result.

Jan 1, 1967

By Manuel Gomez

Low-temperature carbonization product yields for 129 coals representative of 12 Utah coalfields were estimated, using regression equations developed from heating value and proximate and ultimate analysis data. It was shown that yields of char, tar plus light oil, water of decomposition, and gas, as well as the gas volume and the heating value of the gas, could be predicted with reasonable accuracy. Published and experimental results from eight Utah coals carbonized at selected temperatures in the 4500 to 1,000° C range were used to determine the effect of temperature on product yields. Carbonization temperature, heating value) oxygen, and volatile matter of coal appear to be the principal variables influencing carbonization product yields. Data presented show that the heating value and the residual volatile matter in low-temperature char may be predicted using relationships developed from proximate analysis data for 220 coals.

Jan 1, 1967

By A. C. Losekamp, J. B. Conway

Thermal-expansion data for, tungsten, rhenium, tantalum, .molybdenum, niobium, W-25 pct Re, Ta-10 pct W, ant1 Mo-50 pct Re are presented covering the range from room tempature to 2500°C. In these measureMents, made in a resistively heated tungsten tube furnace operating in a helium atmosphere, data for rod and sheet specimens were found to be identical; in addition, arc-cast and sintered tungsten were found to yield essentially identical results. Optical rneasurenlents of thermal expansion .made in any atmosphere other- than vacuum are subject to a refraction error which can be quite substantial. Specimens tested in helium appear shorter than when tested in racuum and hence a special correction factor must be applied to the helium data in order to obtain accurate results. WHILE it is true that linear thermal-expansion data for many of the refractory metals have been measured to very high temperatures, it is also true that except in a few instances the data from various investigators are not in good agreement. This is particularly evident in the case of tantalum and niobium although some tungsten data have been reported which differ by as much as 40 pct from the data of other investigators. Due to the sensitivity of both tantalum and niobium with respect to impurity absorption during exposure to high temperatures, it is probable that this single factor accounts for the majority of the discrepancies in the thermal-expansion data for these metals. However, this same factor can probably not be employed to explain the existing differences in the tungsten data. In all probability, these are due to errors in the measurement technique, to material composition variations, or to changes which take place in the material during the heating process (e.g., additional densifica-tion resulting from heating a sintered specimen above the original sintering temperature). In view of the discrepancies which exist in the linear expansion data reported for many of the refractory metals, the current study was initiated in an attempt to resolve such differences. Also, no high-temperature linear thermal-expansion data were found to be available for several refractory metals. Providing such data was another objective of the current investigation. MATERIALS In this study test specimens were employed in either rod or sheet form and in several instances both arc-cast and sintered material were employed. Material compositions are presented in Table I. Helium gas was fed to the furnace at a rate of about 0.5 SCFH and no special purification procedures were employed. However, the helium contained less than 50

Jan 1, 1967

By J. L. Shultz

Mass spectrometric analyses were obtained for naphthalene and anthracene oils, heavy creosote, and three fractions of a pitch. The average molecular weight, aromaticity, and mean structural unit were determined for each fraction. The investigation of these fractions of coal tar has resulted in semiquantitative data for 38 structural types and carbon number distribution data for their alkyl derivatives. The molecular weights of 10 of these structural types indicate ring systems not previously reported in products from high-temperature carbonization of coal. Two of these structures are poly-nuclear aromatic hydrocarbons, two are oxygen-containing compounds, one contains sulfur, and five are nitrogen-containing compounds.

Jan 1, 1967

By Adrian C. Dorenfeld

[Agitation and transport of slurries have been investigated intensively for the past twenty years. It has been shown (1) that slurries have the properties summarized in Figs. 1, 2, 3, 4, and S. For a detailed exposition the reader is referred to the above reference and the bibliography, which, in turn, have extensive references and bibliographies. An interesting problem with which the senior author has been concerned with is the scab up of power requirements for slurry agitators operating in the laminar region with pseudo plastic materials. Pulps of shaly ores, after various chemical reactions in aqueous leaching systems, are often difficult to settle and filter if agitation is violent. In these cases agitation must be at a minimum, yet prevent [tling] such as in copper uranium ores. This mild agitation is on the laminar region.]

Jan 1, 1967

By Ralph L. Merklin

One of the most commonly employed set of calculations in mill design and research is the material balance, known in wet beneficiation plants, as an Ore and Water Balance. For mill designers, the balance is one of the principal requirements in determining the proper size of launders, pipelines, process equipment, etc. In process development, one of the major goals is the establishment of an optimum balance. The usual procedure for calculating a material balance involves a manual technique utilizing reference tables, pre -obtained data, and a slide rule or desk calculator. With these, the engineer must perform a series of calculations which are repetitious in nature and time consuming. Figure I is the flowsheet of the grinding and flotation circuits for a copper concentrator. The initial ore and water balance was calculated manually and required approximately 24 manhours. Later, a number of changes were made in the balance, each of which required an average of 8 manhours.

Jan 1, 1967

By Mark J. Klein

The behavior of nitrogen in Cr-0.12 at. pct Y was studied in specimens of varying interstitial concentration and thermal history. It was found that soluble nitrogen can be introduced into this alloy by increasing the concentrations of either oxygen or nitrogen. For low nitrogen concentrations the nitrogen in solution is low relative to that in unalloyed chromium. However, the nitrogen in solution increases with increasing nitrogen concentration, approaching that in unalloyed chromium. When the alloy is supersaturated with nitrogen, the nitrogen precipitates readily from solution as a chromium nitride. The stress -induced relaxation of nitrogen is influenced by internal oxidation or internal nitrification of this alloy. THE addition of small concentrations of reactive elements such as yttrium have been found to enhance the low-temperature ductility of chromium.&apos; However, the mechanism by which the ductility is increased is not known. It has been suggested that this effect is caused by a drastic reduction in the concentration of nitrogen retained in solution and therefore a decrease in the number of dislocations locked by nitrogen, a factor that has been associated with an increase in ductility.1,2 However, a change in the type of interstitial precipitate induced by yttrium could also contribute to enhanced ductility of the alloy, since chromium nitride precipitates appear to be embrittling.&apos; In this regard, it has been shown that yttrium scavenges nitrogen in chromium to form YN,4 thus reducing the embrittling chromium nitride phase. However, the change in nitrogen solubility induced by yttrium and the partition of nitrogen between chromium and yttrium nitrides are not known. The object of this investigation is to study the effect of yttrium on the behavior of nitrogen in chromium to obtain information relevant to the mechanism by which scavengers enhance the ductility of chromium. EXPERIMENTAL PROCEDURES The experimental procedures used in this investigation have been described in detail elsewhere.5,6 Wires of Cr-0.12 at. pct Y, 15 cm in length and 1 mm in diam, were drawn from rods 0.6 cm in diam supplied by the General Electric Co. The grain size of the wires after recrystallization at 1150°C was somewhat nonuniform, varying from 0.006 to 0.06 mm in diam. The interstitial analysis for the wires in ppm by weight was about 160 0, 80 N, 12 C, and <2 H. Heat treatments were carried out after encapsulation of the specimens in quartz tubes containing argon. Changes in interstitial concentrations, or interstitial "loading" as it is termed in this study, were generally accomplished by annealing in oxygen, ammonia or methane at 1150°C. The internal friction was measured using a conventional torsional pendulum enclosed in an evacuated chamber. Electrical-resistivity measurements were made at liquid-nitrogen temperature.

Jan 1, 1967

By Clyde M. Pearce

This paper describes the facilities at Pointe Noire, Quebec that Wabush Mines utilizes for the receipt, distribution, stockpiling and shipping of iron ore concentrate and pellets. The main topics to be covered will be: 1. - General description 2. - Concentrate receiving facilities 3. - Conveying circuits 4. - Stockpiling 5. - Vessel loading GENERAL DESCRIPTION The map of the eastern Quebec - western Labrador area as shown in Appendix #1 shows the location of Wabush Mines properties. You will note the Scully Mine located at Wabush Lake, Labrador, 235 miles north of the town of Sept-Iles, Quebec. Our neighbors, the Iron Ore Company of Canada have their properties further north at Shefferville, near by at Carol Lake and at Sept-Iles. To the Southwest, our other neighbors, Quebec Cartier Mining, have their iron ore processing facilities and their terminus on the St-Lawrence at Port Cartier. Concentrates are prepared at the scully Mine by mining, crushing, grinding, concentrating, drying and high tension separation for shipment by rail to Pointe Noire, Quebec. Pointe Noire is situated across the bay from the town of Sept-Iles, Quebec on the North Shore of the St-Lawrence River. The concentrate consists of 66% iron, 2 ¼ percent silica and practically no moisture, permitting the use of specially constructed railroad cars and handling facilities to convert the concentrate into pellets, the final product.

Jan 1, 1967

By Raymond P. Maloney

The Bureau of Mines investigated the White Mountain mercury deposit, in the Kuskokwim River Basin, to better determine the extent of mercury mineralization and to encourage its development by private industry. A program of diamond drilling, augering, bulldozer trenching, and sampling was carried on during four field seasons, from 1960 to 1963, inclusive. Significant amounts of cinnabar, with only trace amounts of arsenic and antimony, occur in dolomite over an area about 4,000 feet long and 1,500 feet wide. The deposit differs from other mercury deposits in the Kuskokwim River Basin by the absence of silica-carbonate and rhyolite intrusives. Small-scale mining was started in 1963 as the result of Bureau investigation and continued during the summers of 1964 and 1965. The investigations indicate that open pit mining might be the most feasible method of working this deposit.

Jan 1, 1967