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By R. F. W. Pease, R. A. Ploc

A scanning electron microscope with a resolving power better then 100Å has been developed for the direct examination of surfaces. This instrument was used to study iron undergoing oxidation at 500°C. It was found that the electron current in the scanning electron microscope was low enough (about 10-atrzp) to have no observable effect on the growth of the oxide. "Armco " iron, when oxidized, exhibited an oxide film whose thickness and whiskey population varied with pain orientation; but purer iron, when oxidized, exhibited no such pain dependence and whisker occurrence appeared to be caused by impurities. UNTIL recently most surfaces of opaque specimens could either be studied with a light microscope or, if higher resolution was required, by viewing a replica of the surface in a transmission electron microscope. Direct electron microscopy of a surface has, in general, proved difficult owing to excessive foreshortening and the poor image quality obtained. The scanning electron microscope, however, offers an alternative method of directly viewing a surface without these disadvantages. At low magnification it offers a much larger depth of focus than the light microscope, and at high magnifications it offers much higher resolution (about 100Å). PRINCIPLE OF THE SCANNING ELECTRON MICROSCOPE A schematic diagram is shown in Fig. 1. The electron optical system consists of a gun followed by a series of lenses which focus the electron beam onto the surface of the specimen. The beam is scanned in a rectangular raster across the specimen surface and, by amplifying the secondary electron current from the 'pecimen, a picture of the specimen surface is built UP sequentially on the face of the display cathode-ray tube. The magnification of such a system is given by the ratio of the scan amplitude on the display cathode-ray tube to

Jan 1, 1965

By D. M. Kehn

A method has been devloped for chromatographic analysis Of the vapor and liquid phases Of a a system containing methane to components having 20 or more carbon atoms. The method uses a windowed equilibrium cell in which volumetric phase behavior of the system can be observed accurately and from which small samples of gas or liquid can be withdrawn for analysis. Analyses are made using two chromatographs, one for the lighter and one for the heavier components in a sample. Combination of the two analyses yields a detailed analysis of the gas or liquid sample. The complexity of the condensate heavy ends is evident from the chromatograms of these fractions, and the predominance of the paraffin hydrocarborn serves as a useful marker in interpreting the chromatograms. The K-values obtained in this analytical method are presented for a high-pressure condensate system and predict closely the observed volumetric behavior of the system. INTRODUCTION Quantitative analysis of hydrocarbons from natural gas reservoirs is necessary for several reasons—to calculate the amount of sales gas produced, to calculate the amount of natural gasoline produced, to plan a liquid recovery system, or to calculate the potential economic value of a reservoir produced under one or more of several different conditions. Analysis of natural gas fluids produced to the surface consists of identifying and computing the mol fraction of each component of the mixture. Although methane is the predominant component, varying amounts of ethane, propane, butane, pentanes and heavier components are also present. Materials containing up to 30 carbon atoms occur in amounts which decrease with increasing molecular weight. However, the quantities of components in the 20 to 30 carbon atom range are usually so small that their importance is negligible, and they are undetect-able in natural gas by ordinary analytical methods. All the components up to those having 20 carbon atoms may sigsficantly affect phase behavior, however. Commonly, only the methane-through-pentane fraction is analyzed quantitatively for each component, while components heavier than Pentane are lumped and repored as "hexane- plus". Expensive, tedious techniques are required for analysis of this fraction. Consequently the detailed analyses needed for prediction of reservoir behavior are usually undertaken only when major gas fields are being developed. The need for complete analyses of condensate systems is apparent when it is recalled that most gas fields are produced by pressure depletion. As the pressure declines, some of the heavier hydrocarbons are lost as liquids which are in the reservoir. In many instances the amount of liquid in equilibrium with the gas phase at high pressure constitutes only 1 or 2 mol per cent of the total system. Flash calculations generally must predict the actual amount of liquid with an accuracy of a few per cent in order to be useful. This retrograde condensation has been understood for years, but accurate correlation methods to permit quantitative prediction of phase behavior in the retrograde region are not presently available. The increasing importance of natural gas has made accurate prediction of phase behavior and composition of produced natural gas streams an economic necessity. The work reported here was undertaken to provide a rapid, economical method for obtaining the vapor-liquid equilibrium information needed to predict accurately the composition of the fluids produced from a gas reservoir throughout its life. TO develop this method, a pressure cell equipped with windows was designed and built for observing the volumes of liquid and gas present at reservoir pressures and temperatures. Use was made of established chromatographic methods for rapid and detailed analysis of both phases. This paper describes the equipment and techniques developed for obtaining vapor-liquid equilibrium data, presents the results of analyses of a condensate system, and indicates the usefulness of these data in predicting hydrocarbon phase behavior. DESCRIPTION OF EQUIPMENT USED The equipment used in obtaining the required information on phase behavior and the complete analysis of hydrocarbon mixtures through C, will be described first, followed by a discussion of the operation of the equipment. It will be helpful, however, to consider first a brief outline of the technique used. A sample of separator gas and liquid is charged to the windowed cell (see Figs. 1 and 2) where volumetric equilibrium phase behavior at reservoir pressures and temperatures can be determined. Then samples of the coexisting phases are withdrawn. The methane-through-pentane fraction is analyzed with a chromatograph equipped with a hot-wire detector, and the pentane-plus fraction is analyzed with a second chromatograph equipped

Jan 1, 1965

By R. H. Ernst, H. R. Ogden, D. J. Maykuth

AT present, no theories exist which allow prediction of the effect of alloying additions on the thermoelectric properties of metals. Nevertheless, Battelle and others1 have observed that, at high temperatures, the peak thermal electromotive-force output (relative to a platinum standard) occurs with metals in Group VI of the Periodic Chart. The authors suspected that this peak was associated with the fact that maximum electronic bond stability is achieved with these metals which have six bonding electrons per atom. On the basis of current electron-concentration theory for transition metals and alloys:' it was surmised that the addition of valency electrons to metals of Groups IV and V (accomplished by the addition of metals from Groups VI, VII, or VIII) should progressively increase the thermoelectric-power output of the resulting alloys until an alloy composition is reached at which the number of valency electrons per atom is six. A further increase in the ratio of valency electrons per atom should then decrease the thermoelectric power. In contrast, the addition of bonding electrons to Group VI, VII, or VIII metals should decrease their thermoelectric power since the electron per atom

Jan 1, 1965

By W. L. Chen

In the United States hydraulic cyclones have been used for thickening, classification and cleaning in coal preparation plants for many years. The cleaning cyclones presently in use are based on using a "heavy medium", such as a fine magnetite and water pulp. The latest addition to cleaning cyclones is the one which uses ?water only?, or simply called "Hydrocyclone". Just as was the heavy medium cyclone, the hydrocyclones were originated in the Netherlands (1, 2). Plants using hydrocyclones were built in Europe (3) and test plants were erected in Canada (4, 5, 6) and India (7). Roberts and Schaefer Company has built four plants using hydrocyclone circuits. One additional plant is in the process of construction.

Jan 1, 1965

By M. E. Volin

Reagent control for optimum concentrate yield was studied by laboratory batch flotation tests simulating the Groveland plant flotation circuit in which a rougher concentrate is cleaned twice. The reagents were a fatty acid collector, a sulphonate collector and sulphuric acid. The study included two types of flotation feed representative of the reground and deslimed tailing from the spiral concentration circuit, one when the ore mineral is predominantly specularite and the other when it is magnetite. The factorial design included three levels of fatty acid, five levels of sulphonate and five levels of H2S04, with the two types of ore in nested blocks, making up a total of 75 tests. Similarity of results and reproducibility were established in preliminary tests. The final tests were performed in random order under closely controlled conditions following the established procedure.

Jan 1, 1965

By William W. Magnus

The Eastern Magnesia Talc Company has always had the problem of adequate storage at its various mines and mills of not only crude ore and finished product but also material in process. An opportunity arose a couple of years ago with the decision to build a new mill at West Windsor, Vermont, (Figure 1) to come as close to providing adequate space for ore and the ground talc in the new plant as money and judgement would allow. Since our engineering staff did not have the time to design and engineer the new facility, an architectural firm with complete engineering staff was retained. Our original thought was to contract all phases of the construction and installation, however, and I think this is a most important point for any small firm such as ours, we found that with good supervision we, as the contractor, could do the job faster and at a lower cost than the construction firms that bid on the work. For some 50 odd years Italian talc has had a virtual monopoly in the body powder area of the cosmetic industry. Due to the purity, superior lubricity and whiteness, naturally occurring in the talc from Italy, no talc in the Western Hemisphere could capture any but a very small part of the market. When the Italian supply was cut off during World War II, the United States' largest consumer of this talc decided that it was time to develop a domestic source of a satisfactory replacement.

Jan 1, 1965

By Jr. Joyce

This report describes sulfatization of nickeliferous laterites from Puerto Rico and the Philippines for recovery of water-soluble nickel and cobalt sulfates. Temperatures ranging from 665 C to 710 C and a 10-percent sulfur dioxide-air reaction gas were employed during batch-roasting tests and during continuous countercurrent treatment in a 2-inch-diameter shaft furnace. A maximum of 69 percent of the nickel and 76 percent of the cobalt were recovered from one sample of Puerto Rican laterite, and a maximum of 96 percent of the nickel and 91 percent of the cobalt were recovered from the Philippine laterite.

Jan 1, 1965

By Harold N. Miller

Lost time and services caused by electrical equipment breakdown or cable faults can often be substantially reduced by the use of direct-current high-voltage testing as a maintenance tool. This paper discusses the relative merits of alternating-current versus direct-current testing, pointing out the advantages in size and cost of equipment and more definitive results achieved through the use of D.C. General principles of direct-current high-volt-age testing, types of testing, methods of performing the actual test and interpreting the results are explained. ?The value of insulation resistance measurements and their relationship to high-voltage testing is discussed. Pinpointing the physical location of a cable defect using a fault locator or thumper is described. Reference is made to several organizations that have effected considerable savings with high-voltage test programs. Introduction T HE past decades have seen great advances in the field of electrical power distribution and application. Motor generators, power-operated equipment, cables, etc., have all gone through various stages of improvement both in efficiency and reliability. Un-fortunately, however, power failures and equipment breakdown still occur -frequently with disastrous effects in loss of time,

Jan 1, 1965

By A. J. Jacobs

THE purpose of this note is to draw attention to a set of tables, recently compiled in Rocketdyne Research Report No. 64-19, under the title "Crystal-lographic Data for Indexing Cubic Twin Reflections and Cementite (Fe3C) Reflections in Electron Diffraction Patterns."' These tables were an outgrowth of electron-diffraction work conducted over the past several years on steels, precipitation-hardening aluminum- and nickel-base alloys, molybdenum, tantalum, and tantalum-base alloys. The first table lists the indices of possible twin reflections for all the possible twinning planes in bcc and fcc lattices. The twin reflections correspond

Jan 1, 1965

By Walter Kahn

Increasing consideration is being given to simplifying traditional methods of tracing pipelines and maintaining required temperatures of stored fluids. Because of their reduction in capital costs, virtual elimination of maintenance. ease of control and "cleanliness"; interest in electrical techniques has accelerated. 1,2 Resistance cable and other heaters have been given some attention. but less well known in the recent introduction of thermal conductive coatings. This paper is addressed to the use of thermal conductive coatings for heating fluid-transport piping and storage tanks. Emphasis will be given to the simplicity, efficiency, and versatility of design and application which their unique properties further contribute to the general economics of electrical heating.

Jan 1, 1965

By W. I. Duvall, D. E. Stephenson

A theoretical solution is given for the energy that is radiated outward when either a cylindrical or spherical cavity located underground in a uniform stress field is suddenly created or enlarged. The method of derivation shows that the stress field in the solid rock surrounding the opening does work on the rock because of elastic displacements that result when the size of the cavity is increased. The amount of this work is sufficient to account for both the increase in the strain energy in the rock surrounding the opening and the seismic energy that radiates outward. Thus, the source of the radiant seismic energy is mainly the gravitational potential energy and not the strain energy stored in the rock. The amount of the radiant seismic energy is directly proportional to the volume of the rock removed from the opening or relieved of stress. Seismic energies from rockbursts are compared with earthquake energies. Also, the amount of gravitational potential energy released by underground explosions is calculated and found to be small compared to the seismic energy generated by the detonation of the explosive. A review of the early literature on rockbursts shows that a number of investigators calculated the amount of energy released by rockbursts. 1-5 However, none of these papers give the formula used to make these calculations or a reference to the derivation of any formulas. The general impression that one obtains from these early papers is that the main source of the seismic energy released by rock-burst is the strain energy stored in the rock before it is fractured. However, a few of the early papers appear to have considered the solid rock at a distance from the mine opening as a possible source of the seismic energy. Recently Black and starfield7 gave a theoretical solution for the strain energy in a stressed plate with and without a circular hole. Also, Press and Archambeau8 gave the theoretical solution for the seismic energy released when a spherical cavity is created in rock subjected to a three-dimensional stress field. Both of the above theoretical papers start with the condition of no opening and calculate the strain energy before and after the opening is suddenly formed. Neither of these papers appear to have calculated the work done by the applied stress field as the cavity is enlarged. The rockburst problem associated with deep mining is concerned with the failure of the solid rock surrounding an underground opening. Therefore, it seems appropriate to consider theoretically the problem of suddenly enlarging the size of an existing opening. The purpose of this paper is to present the theoretical solution for the energy that is available for release as seismic energy when an underground circular tunnel or spherical cavity is suddenly enlarged in diameter. To keep the mathematics as simple as possible, a uniform radial applied stress field is assumed and the rock is assumed to be isotropic, homogeneous and perfectly elastic.

Jan 1, 1965

By R. D. Pehlke, J. V. Gluck

The effect of small additions of silver on the actiziity of zinc in dilute solution with molten bismuth has been determined ill the range 450° to 650°C. Experimental measurements were made in a multi-electrode galvanic cell. All zinc activities showed large positive deviations from Raoult's Law. The results are expressed in terms of the interaction parameter EJ, as defined by Wagner. In the binary Zn-Bi system, Henry's Law was followed at zinc concentrations below 5 mol pct, thus indicating that the binary or self-interaction parameter of zinc in bismuth is essentially zero. The Henry's Law con- THE determination of thermodynamic interaction parameters requires accurate knowledge of solute activities in the dilute-solution region. Dealy and Pehlke1 have summarized the basis for interaction relations, discussed some theoretical implications, and presented a compilation of interaction parameters calculated for molten nonferrous alloys from stant ranged from 2.43 at 650°C to 3.96 at 450°C. The binary zinc activities were consistent with published data for higher zinc concentrations . The ternary interaction parameter ranged from -1.90 at 650°C to -3.30 at 450° C, varying linearly with the reciprocal of the absolute temperature. The negative value for the parameter reflects the fact that addition of silver decreases the activity of zinc in solution with bismuth. data available in the literature. Most of the data were for two-component systems from which only the self-interactions, Ei, could be calculated. Concentration ranges were often such that a considerable extrapolation was required for calculations at lnfinite dilution. The data for ternary systems were quite limited and often unavailable in suitable systematic fashion—thus few values of the parameter e| could be obtained. Knowledge of both the binary and ternary interaction parameters is necessary for the estimation of the activity coefficient of a given dilute solute in

Jan 1, 1965

By Hsun Hu

Based on Kurdjumoiv-Sachs orientation relationship for the fee bee transformation in metals, the jirzal crystal orientation resulting from successive transformations of bee-fee-bee has been analyzed mathematically. There are 528 different variants; many of ther are crystallograpyically equirvalent. Specific examples show that, for equal probability of all the variants, the principal crystallographic axes [100 ], [110], and [111] of the initial bcc crystal can be transformed into vairous axes in the fina1 crystal However, fur each of these principal crystallographic axes, a continuous range of orientation within certain regions of the unit triangle is completely avoided by the finctl Crystals. For uses of higher indices, the final orientations are more uniformly distributed throughout the unit triangle. Results from the PI-esent analysis are in good agreement with preferred Oientations Observed in a zone-meltecl iron bar. THE allotropic forms of iron are characterized by the unusual fact that at both high and low temperatures a bcc structure is stable, whereas at intermediate temperatures (1400" to 910°C) the metal is fcc. Hence, during cooling from its melting temperature, iron undergoes successive phase transformations ofd—? —a with corresponding changes in the crystal structure of bcc — fcc -bcc. while numerous studies have been made in the past of the 1 — a transformation in iron and in various iron-base alloys, no information is available in the literature as to the mechanism of 6 — l transformation and the lattice orientation relationship between these two phases. Experimental difficulties have apparently prevented researchers from undertaking these studies. The laltice orientation relationship between the parent and the new phases of iron resulting from

Jan 1, 1965

By Ralph Hultgren, Prodyot Roy

Manganese vapor pressures from 1250° to 1500°K were measured by conventional Knudsen and torsion-effusion methods in twelve Fe-Mn alloys with compositions from 9 to 80 at. pct Mn. The Knudsen re-sults agveed approximately with previous measurements found in the literature which indicated the solutions were nearly ideal. However, except for the higher manganese compositions, the initial torsion readings indicated much (up to 50 pct) higher vapor presszcres than the Knudsen method. These high readings decreased steadily with time. The results are interpreted as due to depletion of surface concentration of manganese during evaporation. Thus the initial torsion readings are the most nearly correct and Knudsen methods on alloys are to be regarded with suspicion unless it can be demonstrated that diffusion rates are rapid enough to replenish surface concentrations depleted by evaporation. For the lowest manganese contents and highest temperatures, depletion causes initial torsion readings to be too low. FEW thermodynamic data are available for alloys of the high-melting transition metals due primarily to experimental difficulties at the high temperatures involved. Measurement of vapor pressure is one of the most promising techniques to be applied to this problem. From the vapor pressure of a component of an alloy phase, its activity or its partial molar Gibbs energy can be directly calculated. From measurements over a sufficient range of temperatures and compositions the partial and integral Gibbs energies, enthalpies, and entropies may be determined through Gibbs-Duhem integration. For solid phases of variable composition, which commonly are found in alloys, measured vapor pressures are low because of depletion of the surface concentration of the more volatile component as it is selectively vaporized. Diffusion from the interior tends to restore the depleted concentration. The seriousness of the effect depends on the relative rates of diffusion and vaporization. Although depletion has been recognized as a factor,' direct measurements of its rate are lacking and quantitative estimates of its effect on measurements are uncertain. In the present work the vapor pressures above a series of Fe-Mn alloys have been measured by the torsion-effusion method. This method permits a measurement of the vapor pressure of manganese as soon as the sample comes to temperature and continuously throughout the run. The rate of decline of the apparent vapor pressure measures the rate of depletion and the torsion reading at zero time should be correct. At high manganese concentrations (70 and 80 at. pct Mn), the torsion reading remained nearly constant; surface depletion was negligible. There was a slow drop in measured pressure due to bulk loss of manganese from the sample. However, for lower manganese contents, especially at high temperatures, the depletion effect was considerable and the apparent vapor pressure decreased steadily with time. For these alloys the Knudsen method should give pressures which are too low. The measurement of pressure in the Knudsen method cannot be made until enough manganese has been vaporized to be weighable. The Knudsen result is therefore an integrated average between the initial and final vapor pressures. To verify this, conventional Knudsen measurements were also made with results in approximate agreement with previously published Knudsen measurements for these alloys. As expected, for the lower manganese contents the initial torsion readings of pressure were as much as 50 pct higher than the Knudsen. THE APPARATUS The apparatus, shown in Fig. 1, is capable of operating to temperatures up to 2000°K. A vacuum of 5 x 10"6 mm Hg can be maintained. Temperatures were measured to +3° by a W-Re thermocouple placed in the dummy cell, N. The torsion cell consisted of two alumina crucibles with holes in their covers. They were placed in the molybdenum holder shown suspended from the torsion wire. Rectangular torsion wires (1 by 4 mm) were found to have superior sensitivity and less residual distortion than circular (2-mm-diameter) wires. The precision of angular measurement was found to be *0.025 deg; the variation is no doubt due to temperature fluctuation and vibration. For the Knudsen experiments the alumina cell was set on the support, N. SAMPLE PREPARATION 800-g samples were prepared by melting together electrolytic iron and electrolytic manganese and pouring the melt into a water-cooled copper mold. Melting and pouring were done under a helium at-

Jan 1, 1965

By K. Barron

The glass insert stressmeter, or photoelastic stressmeter, is an instrument designed to determine stress changes occurring in rocks. It has several potential advantages over other such devices in that it is a biaxial device, it is simple and it is cheap to make. The object of this study was to assess the behaviour of the meter under biaxial loads and to examine some of the problems associated with measurement and interpretation of the fringe pattern. This assessment has been carried out by comparing theoretical and laboratory behaviour of the meter. It has been shown that: a) There are certain optimum measuring points in the meter at which measurements should be made for best accuracy. The position of the points depends on the ratio, n, of the biaxial stresses. b) The meter&apos;s sensitivity can be assumed to be independent of the rock modulus E provided that the rock modulus is < 2.5 x 106 psi and not, as previous workers have assumed, if E < 5 x 106 psi. c) There are several methods of separating the principal stresses; some of these are unsatisfactory. A new method is proposed and discussed. d) The meter sensitivity decreases as the ratio of the biaxial stresses approaches unity; the accuracy thus also decreases. e) The axes of symmetry of the fringe pattern give an excellent indication of applied stress direction. f) Laboratory calibrations are in good agreement with theory. The glass insert or photoelastic stressmeter is an instrument designed to determine stress changes occurring in rocks. It has several potential advantages over other such devices in that it is a biaxial device, it is simple and it is cheap to make. This stressmeter has been described in detail.l,2 Basically it is a hollow glass cylinder that has at one end a light source and filters producing circularly polarized light. The glass cylinder and source are grouted into a borehole in rock and the face of the cylinder is viewed through a quarter wave plate and an analyser. If, after installation, a stress change occurs in the rock, then a distinct colored isochro-matic fringe pattern is seen in the meter. The fringe order at any point in the meter can be determined by counting the fringes and measuring the fractional fringe orders by the Tardy compensation method. The relation between the fringe order at any point and the applied stress change can be determined either by calculation or by calibration. The object of this study was to assess the behavior of this stressmeter under biaxial loading conditions and to examine some of the problems of interpretation of the fringe pattern. THEORY Hiramatsu et a14 have determined the stress distribution in a hollow cylindrical inclusion in an elastic host material when subject to uniaxial stress. Using this solution, the biaxial case of stress p in the x direction and stress q in the y direction (Fig. 1) can be solved by superposition. This has been done in Appendix 1. It is shown that the principal stress difference (s1 -s2) at any point (r,?) in the cylinder is given by:

Jan 1, 1965

By John W. Thatcher

A demountable X-ray tube vacuum spectrograph was designed by the Bureau of Mines for the determination of long-wavelength X-ray spectra from the light elements. This instrument was operated for both secondary and combined primary-secondary excitation of the aluminum K-series. There was an increased analytical sensitivity for elements in period 3, and an indication that with improved X-ray tubes or direct election excitation of the sample, X-ray determination of elements in period 2 is also possible.

Jan 1, 1965

By M. N. Shetty

LARGE copper whiskers (-100 p) of 11111 orientation were tested in a floor-model Instron testing machine, at liquid nitrogen temperature. (Testing methods will appear elsewhere.) Whiskers deformed by twinning after some initial deformation. A load-elongation curve at the onset of twinning is reproduced in Fig. 1. Twinning was confirmed by taking a back-reflection Laue picture, using a slit colli-mator, which showed distinct splitting of reflections. The tensile stress reached just before twinning is about 1.4 x 107 g per sq cm (-7.0 x106 g per sq cm—resolved shear stress) which drops to 1.2 x107 g per sq cm (-6 x 106 g per sq cm—resolved). This twinning stress is about five to ten times larger than the value for bulk single crystals of copper deformed at 77°K (-106 g per sq cm—resolved). Twinning models based on Cottrell-Bilby&apos;s pole mechanism are discussed in detail by Venables.&apos; In the present work a mechanism based on the idea of failure of a Lomer-Cottrell barrier by recombination will be proposed. An L-C barrier may fail either by recombination or by dissociation.3 Fig. 2 provides the necessary information. It shows that the stress necessary to break such a barrier is about 1.8 x 107 g per sq cm by recombination and 4 x 107 g per sq cm by dissociation at 77°K. The twinning stress reached by whiskers is comparable to the stress level required for failure of an L-C barrier by recombination. (Stroh himself points out that his calculations should not be taken too literally.) We consider a segment of the L-C dislocation which has recombined (AB in Fig. 3) over a length to form the total dislocation which then glides in the

Jan 1, 1965

By T. K. McMahon

Formally, a mathematical model could be defined as: A set of equations whose solution will approximate the response of a physical process or system to a set of stimuli which appear as parameters in the equations. The purpose of a mathematical model is to permit the rationalization of experience to proceed by simulation rather than by physical experimentation. In the application of digital computer control to an industrial process, the mathematical model of the process (subsequently called the process model) is needed to calculate the present process performance from the measured variables and to predict the response of the process to a control change. Functionally, the cardinal element in process model development is a concise set of control objectives. These, besides implicitly defining the boundaries of the system to be modeled, will determine the accuracy demanded of the model its nature: dynamic or steady-state, and so forth, The objectives should explicitly define what process efficiencies, production rates, qualities are to lie within the scope of the computer control project, thereby providing a basis for simplifying assumptions in the development of the model. This requirement, a limited set of control objectives, is so often disregarded in formulating industrial control problems that its repetition can scarcely be avoided.

Jan 1, 1965

By James F. Neill, O&apos

Brown iron ore resources in Barbour, Butler, Crenshaw, and Pike Counties were investigated in a drilling program and geological study by the Federal Bureau of Mines in cooperation with the Alabama Geological Survey and the University of Alabama. The aggregate footage drilled was 18,010 linear feet. When developed, reserves of 12,664,000 long tons of crude ore were indicated, containing from 26.9 to 29.0 percent iron and 0.2 to 1.6 percent manganese under a maximum overburden of 40 feet. Total inferred crude ore for the four counties was calculated to be 827,700,000 long tons. Beneficiation of samples by simulated log washing and use of a 1/8-inch screen yielded from 46.8 to 51.7 percent iron and 0.2 to 2.6 percent manganese. Screen-test studies indicated no appreciable interlocking between the iron and manganese minerals and the waste particles of materials retained on a 200-mesh screen. Clay was prominent in micron-size slimes. Silica was deleterious in the minus 20-mesh size. While an indicated 2,198,000 dry long tons of usable iron ore can be recovered, sink-and-float tests show that it may be possible for 4,654,000 dry long tons to be recovered by other than log washing. However, applicable commercial processes have not been demonstrated.

Jan 1, 1965

By Don M. Jackson

The techniques for the growth and controlled, graded doping of silicon epitaxial overgrowth layers were established. Grading of- impurities such as arsenic or boron in arbitrarily chosen profiles oiler four orders of magnitude (from I X 10Lg to 1 X 10L5 cm) was accomplished. The graded structures were grown in a stepwise manner where in the profiles were approximated by growing many separate layers with small doping-level changes between layers. Masked-area growth of silicon through windows in a SiO2 masking film was acconiplished through the simultaneous injection of HCl gas 102th Sic14 in the epitaxial reactor. The HCl served to inhihit the growth of silicon on the Sz02 surface, and also to control the cross-sectional profile of the silicon mesas. silicon from the substrate was etched out through the windows, and then epitaxial material was used to fill the holes hack in to form planar diodes. Simullaneous HCl injection was adapted to control the cross-section profile of the hack-filled regions. Arsenic-huried regions beneath in te- In recent months, the epitaxial growth process in semiconductor materials technology has evolved into a complex system directed at both material improvement for better monolithic integrated-circuit characteristics and the development of new silicon structures for future integrated-circuit needs. The advent of high-temperature HC1 gas etching1 grated-circuit transistors reduced V(SAT) by slightly more than one third, bringing this parame-ter to that of an isolated component transistor. When arsenic was diffused into the starting sub-stvate, it was necessary to remove any excess arsenic in order to avoid excessive audodoping of the subsequent epitaxial layer. Oxide isolation of single-crystal regions in a substrate provided complete electrical isolation of integrated-circuit components, thereby eliminating parasitic capacitance which is inherent in standard integrated-circuit processing. The process involved the etching of deep mesas on silicon Wafers, the formation of an oxide over the mesa surface, and then the deposition of several mils of polycrystalline silicon over the oxide. The original substrate was lapped and polished allay until the mesas were left isolated in the polycrys-talline matrix. The Final components were fabri-cated in the single-crystal islands. Speed and power-handling capabilities of standard circuits were improved through the process. wherein work-damaged material is removed from the surface of the silicon wafer just prior to the silicon deposition step has made it possible to grow silicon films with structural quality that approaches that of the substrate. HBr used in the same volume ratio as HC1 etches silicon at the same rate and with the same results as HC1. Recent developments in epitaxial materials technology have occurred in the areas of precise doping control, buried prediffused regions between over-

Jan 1, 1965