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By C. Q. Cupps

n view of increased interest in secondary recovery of oil in the Cut Bank field, Montana, a review has been made of unpublished data obtained during a 1943-44 study of reservoir oil characteristics in this field. Considerable uncertainty was attached to interpretations of subsurface oil sample analyses from six Cut Bank zone wells, one Lander sand well, and one Moulton sand well, because of adverse sampling conditions and wide range in the data. Much of this uncertainty has been removed by this review which has shown two of the Cut Bank zone samples and the Moulton sand sample to be representative of the reservoir oils. Estimates of original reservoir oil characteristics derived from differential-liberation analyses of these samples show that the oil in the Cut Bank zone was initially saturated at the gas-oil contact pres-sure, 750 psia, and the oil in the Moulton sand was undersaturated with a saturation pressure of only 380 psia. The rest of the samples were indicated to be nonrepresentative of the reservoir oils because of a disproportional vaporization of heavier components of the solution gas. The vaporization of these components is believed to be a cumulative effect of contact of the oil with bypassing, light-gravity gas which had been liberated at higher pressures from solution in oil farther back in the formation, or which had come from the gas cap, rather than from the singular effect of gas evolution caused by excessively low bottom-hole pressures. Change of oil composition caused by the latter was found to conform closely to that occurring during a differential liberation of gas in the laboratory.

Jan 1, 1967

By Sarkis G. Ampian

Extraction of alumina was correlated with the sinter and leach products from the lime soda sinter process for anorthosite. The effect of composition and grain size of reactants, time and temperature of sintering, and techniques of sample preparation were investigated. Greater than 90 percent Al2O3 extractions were obtained from dry-mixed minus 200-mesh anorthosite sinter mixes having mole ratios of CaO/SiO2 = 1.8 and Na2O/Al2O3 = 0.8. These sinter mixes were briquetted at 15,000 psi and fired between 1,200° C and 1,320° C for 20 to 60 minutes. The sinter phases that contribute to low alumina recovery were determined by X-ray diffractometry, optical microscopy, and electron probe X-ray spectrography. The mechanism of the sintering reaction was investigated by high-temperature X-ray diffractometry. The contrast in the lime soda sinter process for clays and for anorthosites are discussed. Explanations and suggested solutions are presented for problems such as gelation and variable alumina recovery encountered by previous investigations.

Jan 1, 1967

By Jr. Koch

As a means of investigating the distribution and variability of gold in ore from the Homestake mine, Lead, S. Dak., the Bureau of Mines performed a designed sampling experiment, and assay results were statistically interpreted. Fifty-six feet of diamond-drill core from five boreholes was sawed into l-inch-long cylinders, which were sampled randomly and were assayed. Analyses of variance of the assay results were used to compare and assess the different types of variation: within drill holes, among paired drill holes, among unpaired drill holes, and among furnace runs. The extreme variability in gold mineralization found is the natural variability on the smallest scale that can be detected by fire assay; most of the variability is associated with among-feet rather than within-feet sample intervals. Because of the extreme variability, one-half of the gold is in 3 percent of the samples.

Jan 1, 1967

By I. C. Edwards, G. E. Agar

INTRODUCTION Many research efforts over the past years have been devoted to the study of energy consumption in comminution and the characteristics of the broken material. The old "laws" have been superseded by more general methods of analysis1,2,3 but these methods have not received much attention outside the laboratory. The work to be described here was done in order to obtain scale-up information on wet rod milling of sylvinite. EXPERIMENTAL A 30 x 51 in. Denver rod mill with a scoop feeder was used for these tests. Ore was fed from a variable speed screw conveyor into the feed box along with saturated brine. The mill was filled to approximately 45% of its volume with 2400 lbs of a mixed rod charge. The minimum possible feed rate was 2.5 tph and the practical maximum for this mill was 8 tph. Individual tests were run by setting the solid feed rate, then adjusting the brine flow rate to give the desired pulp density. After steady state, as evidenced by constant discharge pulp density, had been reached, samples of the discharge were taken at 15-minute intervals. These samples were filtered, washed with alcohol, dried, then screened on Tyler screens using a Ro-tap shaker. The sylvinite feed was regular plant feed that had been scalped at 20 mesh and was tapped from the coarse ore bins. It had been previously passed through a roll crusher set at 3 inches and after scalping was essentially minus 1 in. plus 20 mesh. RESULTS The screen analysis of samples from each series of tests was plotted on double logarithmic scale paper to determine the reliability of the series. In some cases, a faulty sample or screening procedure dictated that the results of one test be discarded. The criterion is a simple one — if the slope of one plot was noticeably different from the others in the series, it was discarded. The only cases that caused difficulty were those in which the brine was not thoroughly displaced from the solids. When this occurred agglomerates were easily identified on the screens and the whole of the sample was retained on 3 or 4 screens. There were no border line cases. The number N given in Table 1 is the number of size analyses that were pooled to form the data shown in Fig. 1. While examining the reliability of the sizing and sampling by plotting the data, it became apparent that there was no significant difference between grinds made at 50 and 60% solids. For the analysis given here, these tests were regarded

Jan 1, 1967

By Franklin D. Slagle

Porosity and bulk-and sand-grain-density values were determined for 2,040 core samples of 30 formations from 47 wells in New York, Ohio, Pennsylvania, and West Virginia, and are compiled for petroleum industry use in well-log evaluation and geologic studies.

Jan 1, 1967

By Jr. Fish

As a part of a study of iron are resources in the Appalachians, 9 diamond drill holes aggregating 1,580.7 feet were drilled in a portion of the Butt Mountain area of northeastern Giles County, Virginia. Three hematitic sand-stone beds were intersected in the Clinton formation but only one was consistent in thickness and grade in all 9 drill holes. This bed averages 18.9 percent iron over an average thickness of 24 feet. The drill cores were logged and chemical analyses were made on 161 individual samples and 22 composite samples. Beneficiation studies were made of three composite hematitic sandstone samples each representing a separate bed containing 14.6, 19.8 and 20.0 per-cent iron. Major mineral constituents of the samples were hematite, quartz, and sericite.

Jan 1, 1967

By K. E. Stanfield

Oil-yield results are presented for 65 oil-shale sections in Piceance Creek Basin, Colorado, sampled during the period 1957 through 1963. Including previously published data, oil-yield results for 203 sampled sections have now been released by the Bureau of Mines to aid in appraising the shale oil potential of the basin. Oil yields of core samples (135 sets) were regarded as reliable bases for appraising the Mahogany-zone interval, but only 5 sets of cores sampled the deeper, lower-zone oil shales. Drill cuttings (68 sets) sampled the lower-zone oil shales, but their oil yields are principally indicative and should be confirmed by analyses of cores. More complete core sampling of the lower-zone oil shales is needed.

Jan 1, 1967

By James A. Wasson

The Mitchell and Berea sands were cored and logged in Fred Link well K-l, Lower Newport field, Washington County, Ohio. Core and reservoir fluid analyses and available field data were studied to determine if these sands could be successfully waterflooded. The results of the study indicate that there is insufficient oil in place to form an oilbank in either the western Mitchell pool or the Berea sand, and that no commercial recovery of oil by waterflooding can be obtained in these reservoirs.

Jan 1, 1967

By P. A. Peach, W. H. Gross

The modern economic geologist in Canada is well equipped to apply geological, geochemical or geophysical techniques in the exploration for ore. Recently, great advances have been made in geophysics and geochemistry, and a large number of new orebodies have been discovered by these methods. An attempt is made in this paper to show that there has also been a considerable advancement in geological knowledge and that the most effective application of geophysics and geochemistry often occurs in areas already considered geologically favourable for the occurrence of ore. Ali exploration methods sooner or later suffer from diminishing returns. Therefore, as time goes on, one can expect to see the application of some of the more subtle or refined geological techniques that are presently being developed.

Jan 1, 1967

By William F. List, Marvin A. Schuster

Monolithic electrooptical mosaics of 2500 photo-transistor elements with internal row and surface column interconnections have been fabricated by epitaxial-planar diffsion techniques. Unique access to any elemed of the mosaic is provided through one of the fifty X and one of the fifty Y external leads. The sensor mosaic can be used for imaging applications and has a 1:1 aspect ratio, a resolution of 100 lines per in., a dynamic range in excess of lo3, a sensitivity of 0.5 per pw, element response within a 2:l range over 75 pct of the mosaic, and a minimum detectable signal of the order of 10-' w. Design considerations which ilnpose particclar fabrication yequirements are disctussed along with some of the problems peculiar to the epitaxial and planar-dijfision techniqes by which this device is fabricated. The solid-state silicon monolith has an imaging area of 0.5 by 0.5 in. and an element center -to- center spacing of 0.010 in. J monolithic solid-state electrooptical device has been developed as the photon-sensing mosaic for use in an image-converter system.' This system is the solid-state equivalent of the vidicon and can image radiation in the visible and near-infrared regions of the spectrum. The electrooptical image converter has the desirable size, weight, reliability, and low-power characteristics inherent in solid-state devices. It is read out by direct-wire means rather than by beam-scan techniques. The packaged unit is shown in Fig. 1. A selection of material for the sensor was based on considerations of both reliable fabrication techniques and material spectral response. Silicon was selected both for its response from the lower end of :he visible to the long-wavelength cut-off above 11,000A and for its well-developed epitaxial planar-diffused technology. The electrical image is composed of M x N discrete information bits with each bit emanating from one of the individual phototransistor sensors. The interconnected mosaic concept was introduced to provide a structure which is both manageable in its number of leads and compatible with conventional viewing systems which accept XY data. Interconnections along the Y direction are provided by internally diffused strips, while interconnections along the X direction are formed by vacuum-deposited metal surface bars. Unique access to any individual element of the M x N mosaic is available through one of the M and one of the N external leads. PHOTOTRANSISTOR DESIGN A phototransistor structure2 was selected for the discrete photon detectors of which the mosaic is com- posed. Basically, the mode of phototransistor operation is such that incident quanta are absorbed in the base area of the element where they generate electron-hole pairs. If the electrons are liberated within a diffusion length of the depletion region around the collector junction, they will diffuse to this depletion region and be swept across the junction where they account for a small component of the photocurrent. Similarly, the holes which are created within a diffusion length of the emitter junction will diffuse to this region where they forward bias the emitter and so induce injection of minority carriers into the base. This accounts for the substantial transistor photocurrent. This mechanism of operation implies several design and fabrication goals for the individual sensor elements: high electrooptical conversion efficiency, sufficient carrier lifetime in the base regions, and a maximum volume in which photons can be absorbed within a diffusion length from the depletion layer about the junction. Moderately high transistor gain is desirable to permit readout at low light levels; however, very high gain has a deleterious effect on mosaic dynamic range. The mosaic must also be characterized by good uniformity of element response as well as by good isolation between elements. The above set of conditions imply that junction depths must be optimized with respect to photon ab-

Jan 1, 1967

By C. W. Drake, J. H. Walsh

"The Canadian Carbonization Re-search Association was formed during 1965, with seven founding members representing four integrated steel companies, two coal companies and one high-temperature tar processing company. The purpose of this paper is to review the circumstances which led to the formation of this new research association and to discuss its general objectives. Also discussed will be the organization of the Association, the nature of its relationship with the Department of Energy, Mines and Resources in the early stages, and some of the technical programs which have now been initiated."

Jan 1, 1967

By N. A. Gjostein

The formal descnption of the decay of an isolated scratch can be written in terms of an appropriate Fourier integral. With the application of certain approximations, this description leads to the second-moment analysis developed by King and Mullins. It is shown that the second-moment analysis does not adequately describe the behavior of a decaying, isolated scratch, and that it is difficult to obtain internally consistent values of the surface self-diffusion coefficient, D,,from this analysis. This inconsistency arises from contributions of higher-order moments to the decay process. Two new analytical methods, based on the Fourier integval representation of a scratch profile, have been developed for determining values of D, from the decay kinetics of isolated scratches. In the profile-matching method, a given initial profile is resolved into its Fourier components, the components are allowed to decay exponentially over an annealing time interval, At, and finally they are synthesized to form a decayed profile. The predicted profile is adjusted to fit the experimental profile by varying only the parameter, D,At; the contribution from volume diffusion is directly taken into account and the integrals involved in the Fourier analysis are evaluated by numerical integration on an electronic computer. In the kinetic method, the widths, W, of a series of predicted profiles are determined for various volume-diffusion contributions, and the results are plotted in the form W vs DSAt. For a fixed ratio of surface to volume diffusivities, R, these plots are linear; the slope of the lines increases as R decreases. A simi-lar analysis can be performed on the depths of the predicted profiles. In this case, plots of (l/df3 vs D,At are found to be nonlinear. The proper value of Ds is found by superimposing the data for the experimental widths and depths on Plots of this kind and adjusting Ds until a fit is obtained with the line having the appropriate value oj R. An analysis of the slopes of these plots for R —= (surface diffusion only) reveals that they do not give the correct value, 2276, for width tf second-moment standard profile. This finding allows one to modify the second-moment analysis in such a way as to obtain internally consistent values of Ds. ThERE are several processes, involving a flow of matter along a surface, due to gradients in curvature of the surface, that may be used to determine the surface self-diffusion coefficient, Ds. These processes are commonly known as 1) thermal grooving, 2) single and 3) multiple scratch decay, 4) blunting of field-emitter tips, and 5) sintering. In this series of papers, the first three of these processes are examined in detail in an attempt to subject the phenomenological theories governing these processes to a critical test and, furthermore, to make a critical comparison of the values of D, obtained from these techniques. Although the thermal grooving technique has been established'' as a reliable method for determining D, , this has not been the case for the process of scratch flattening. Mullins and coworkers374 have proposed phenomenological laws governing the growth of the width and the decay of the amplitude of an isolated scratch, but only in one study5 has the width-growth law been supported by experimental evidence. In paper I of this series detailed experimental evidence is presented that points up the deficiencies of the second-moment analysis; the origins of these deficiencies are also discussed. Following this development, some new analytical procedures, based on representing the scratch profile by Fourier integrals, are presented as a means of obtaining reliable values of D, from the kinetics of the scratch-flattening process. Further applications of the Fourier integral approach are reported in papers 11' and 111,~ where the method has been useful in interpreting the anisotropy of flattening rates of isolated scratches (paper 11) and in describing the multiple scratch decay process (paper 111). THEORY OF SCRATCH DECAY Following ~ullins" approach we consider an arbitrarily shaped scratch profile, Fig. 6, at some time, t. The profile is designated by a function z(x,t) which can be expressed in terms of a Fourier integral as follows:

Jan 1, 1967

By Robert E. Wood

The compressibility factors, Z, of helium, nitrogen, and helium-nitrogen mixtures in the three-dimensional space of temperature, pressure, and gas composition have been related to the Leiden form of the virial equation of state. The dependency of virial coefficients through the fifth on temperature and gas composition has been established for the temperature range 133.15° to 748.15° K. Compressibility factors, Z, have been computed from the equation of state and tabulated as functions of gas composition, pressure, and temperature. Tabular values of Z are presented for 30.00 through 100.00 percent helium for temperatures from 240° through 700° R for pressures from 14.696 through 3,050 psia and for temperatures from 720° through 1,300° R for pressures from 14.696 through 1,500 psia. Tabular values of Z are presented at increments of 5.00 percent helium and 20° R, and, for pressures greater than 50 psia, at increments of 50 psi.

Jan 1, 1967

By Alla D. Mah

Heat content and entropy data at high temperatures were obtained for cuprous oxide (Cu2O) and cupric oxide (CuO). Experimental results and smooth values are reported. Equations are given for heat content increments and heat capacities above 2980 K. Low-temperature heat capacity data were obtained for cuprous oxide. Evaluation of the 2980 K entropy gave, S°298.15(Cu2O) = 22.08 ± 0.10 cal/deg mole. Heat of formation values were determined for cuprous and cupric oxides. The values are: AH°298.15(Cu2O) = -40,830 ± 300 cal/mole, and AH°298.15(CuO) = -37,230 ± 150 cal/mole.

Jan 1, 1967

By K. Mukherjee

A quasi-thermodynamic calculation is presented for estirt~ating vacancy Parameters in fcc metals. For fcc metals the equilibrium vacancy concentration at the melting point can be approximated by a constant mole fraction. The Gibbs free energy of formation of the vacancies can then be expressed as a simple function of the absolute melting temperature alone. From this description the formation energy Ef, the vibrational entropy Sv, and the formation volume of a vacancy can be calculated in terms of known thermodynamic parameters. The calculated values are in good agree-rnent with available experimental results. IT appears that many of the physical parameters associated with lattice defects can be empirically related to thermodynamic melting parameters.'-7 Besides the implicit correlations between melting phenomenon and point defects, the melting temperature itself at atmospheric pressure can be used as a reference temperature for the purpose of comparison of vacancy concentrations in a given crystal class. The concentration at the melting point then corresponds to the maximum vacancy super saturation in the crystalline state at a fixed pressure. For pure fcc metals such as Au, Cu, Al, Ag, Pb, and Pt the mole fraction of vacancies at the melting point8 is of the order of 10*"3 to 10"1. The equation expressing the equilibrium vacancy concentration at the melting point contains three parameters: the formation energy, the vibrational entropy, and the absolute melting temperature, see Eq. [2]. Since these three parameters cover a wide range of values8 in the above-mentioned metals, it can be assumed that in other fcc metals, for which no reliable data are available, the mole fraction of vacancies at the melting point most likely lies in the range 10~3 to lO"4. This is then the basis of the calculations described in this article. Within this range the mixing entropy can be linearized and the vibrational entropy, the formation energy, and the vacancy formation volume can be calculated in terms of known thermodynamic constants. 1} LINEARIZATION OF MIXING ENTROPY The Helmholtz free energy of a crystal containing n vacancies at the melting point can be writteng as where Ef, T,, k, and S, are the formation energy of a vacancy, the absolute melting temperature, Boltz-mann's constant, and the vacancy formation entropy, respectively. After applying Stirling's approximation in Eq. [l] and minimizing with respect to n where (n/N), is the equilibrium vacancy concentration in mole fraction at the melting temperature at 1 atm pressure. If instead of setting (6~/6n) = 0 immediately after Stirling's approximation in Eq. [I], the configurational partition function is simplified, then some useful and significant results can be obtained by utilizing the experimental inforrnation After applying Stirling's approximation and rearranging is plotted as a function of (n/N) in Fig. 1. The points, not all of which are shown, are fitted by a straight line substituting from Eq. [5] into Eq. [I] and minimizing with respect to n combining Eqs. [6] and [2] It must be emphasized that Eq. [7] is only a crude approximation based on an oversimplified model of

Jan 1, 1967

By Raynor Linzey, Karl M. Busen

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

Jan 1, 1967

By Stanley A. Feitler

This Bureau of Mines report deals principally with the resources and economic aspects of feldspar in the United States east of the Mississippi River. Although in a strict sense, all phases of the feldspar industry affect its economic structure, emphasis in this study is on supply, demand, and marketing. Although feldspar was originally mined for use in the manufacture of pottery and other ceramics, the glass industry, which began to use feldspar in the mid-1920's, now consumes more than half of the annual output. Most mining is open cut, and the methods used are similar to those used in mining crushed b stone. Excess plant capacity has been chronic, and production is usually about 30 percent of capacity fur the industry as a whole. Since 1947, feldspar consumption has grown more slowly than the average for all U.S. industry. This has fostered intense competition, especially for the glass market. Prices have not kept pace with inflation, and profits are small. The trend of consumption through 1970 for glass feldspar is expected to be upward; less rapid in consumption of ceramic feldspar is anticipated.

Jan 1, 1967

By Alexander E. McHugh

A study of some variables affecting the recovery of molybdenum from oxidized molybdenum minerals was made. The effects of variations in contact time, temperature, pulp density, particle size, and solvent concentration on the recovery of molybdenum using acid and alkaline solvents were investigated. Chemical analyses, screen analyses and microscopic examinations were made and the presence of important elements determined. A hydrometallurgical method was developed to recover the molybdenum from the oxidized molybdenum ore by simultaneous dissolution of the molybdenum with sulfuric acid, adsorption on activated charcoal and flotation of the charcoal. The molybdenum was extracted from the activated charcoal with sodium hydroxide, precipitated with calcium hydroxide as calcium molybdate and this regenerated sodium hydroxide for additional stripping. A solvent extraction method, using mines, was also studied to recover molybdenum from both alkaline and acid molybdenum solutions. Satisfactory results were obtained.

Jan 1, 1967

By Robert W. Ageton

The Bureau of Mines investigated the in situ vertical component of the rock stress in the rib of the haulage drift on the 6100-level of the Star mine, Burke, Idaho, using the flatjack and borehole deformation methods. The estimate of the vertical component of stress about 2 feet into the rib at a station along the haulage drift on the 6100-level of the Star mine by the flatjack method is approximately 5,875 psi, whereas the borehole deformation procedure at this station yielded a value of 5,500 psi for the same depth into the rib. The test zone is approximately 5,625 feet below the surface.No attempt was made to extrapolate stress estimates beyond the depth of the flatjack installation.

Jan 1, 1967

By F. V. Shallcross

Physical properties of thin films of CdS and CdSe formed by vacuum deposition onto glass sibstrates have been studied as a function of deposition and processing conditions. The crystallinity and surface features of CdS films were examined using electron microscopy and electron and X-ray diffraction techniques. The films were poly crystalline; the preferred orientation and crystallite size increased with film thickness, substrate temperature, and deposition time. The CdS films consisted primarily of hexagonal-phase material, in contrast to similarly prepared CdSe films which have previously been observed to contain mixtures of cubic and hexagonal phases. As-deposited CdS films showed no major dependence of Hall mobility on crystallite size or degree of preferred orientation. Hall mobility and carrier concentration in CdS and CdSe .films were measured at various temperatures; both parameters increased with temperature and yielded activation energies which depended on fabrication conditions. Surface-desorption phenomena and overcoating of the semiconductor with SiO affected the observed electrical properties significantly. THIN films of cadmium sulfide1,2 and cadmium sele-nide3,4 have been employed by various workers as semiconductors in the insulated-gate thin-film field-effect transistor, known as the TFT. These devices are most commonly made by vacuum deposition of all materials onto an amorphous substrate such as glass. A knowledge of the microstructure and electrical properties of semiconductor layers used in the thin-film transistor is essential in order to form a realistic model for the device and to improve its performance, reproducibility, and reliability. This paper will describe studies of the physical properties of vacuum-deposited CdS and CdSe films prepared under various conditions. Structural characteristics examined in- cluded phases present, crystallite size, nature of preferred orientation of crystallites, surface roughness, and structural homogeneity throughout the film thickness. Electrical properties measured were Hall mobility and conductivity and their dependence on temperature and ambient. Thin-film properties are affected by many fabrication parameters including purity and physical form of evaporant, deposition rate, film thickness, design and temperature of the evaporation crucible, geometry of the deposition chamber, nature of the residual atmosphere, composition and temperature of the substrate, and details of postdeposition processing. PREPARATION OF FILMS In this work the semiconductor films were deposited in a conventional oil-diffusion-pumped system with pressures in the 10-8 torr range. The CdS evaporant was obtained from the Eagle-Picher Co. as a high-purity coarse-grained crystalline powder; the CdSe was a high-purity sintered powder supplied by the Harshaw Chemical Co. The evaporation crucible was a resistance-heated molybdenum-wire basket coated with aluminum oxide and filled with a quartz wool plug at the top. The source to substrate distance was usually 10 cm. This region was enclosed by a Pyrex inner cylinder. The substrate was heated with an overlying Pyrex plate coated with tin oxide. The substrate temperature was controlled using a thermocouple attached to the lower side of the heater. This thermocouple was calibrated against another thermocouple attached to a dummy substrate and by observation of melting points of various metal films deposited in the system. The substrates were polished borosilicate glass plates and conventional glass microscope slides. Substrate preparation included cleaning with an ultrasonically agitated detergent bath followed by isopropanol-vapor de-greasing. Film thickness was measured interferomet-rically during and after deposition. STRUCTURE OF CdS FILMS Structural studies were performed on CdS films using electron diffraction, electron microscopy, and

Jan 1, 1967